JAERI-Conf 99-009

JP9950621

PROCEEDINGS OF THE THIRD JAERI-KAERI JOINT SEMINAR ON THE POST IRRADIATION EXAMINATION TECHNOLOGY

MARCH 25-26,1999, JAERI OARAl, JAPAN

September 1999

Japan Atomic Energy Research Institute WffiftiS (=f319-1195

(T319-H95

This report is issued irregularly. Inquiries about availability of the reports should be addressed to Research Information Division, Department of Intellectual Resources, Japan Atomic Energy Research Institute, Tokai-mura, Naka-gun, Ibaraki-ken, 319-1195, Japan.

©Japan Atomic Energy Research Institute, 1999 JAERI-Conf 99-009

Proceedings of The Third JAERI-KAERI Joint Seminar on Post Irradiation Examination Technology March 25-26, 1999, JAERI Oarai, Japan

Department of JMTR

Oarai Research Establishment Japan Atomic Energy Research Institute Oarai-machi, Higashiibaraki-gun, Ibaraki-ken

(Received August 4, 1999)

Between the Department of JMTR of the Japan Atomic Energy Research Institute (JAERI) and the Nuclear Fuel Cycle Research Group of the Korea Atomic Energy Research Institute (KAERI), it has been periodically carried out the collaboration on technical information exchange by specialists and scientists, under the Arrangement of the Implementation of Cooperative Research Program in the Field of Peaceful Uses of Nuclear between JAERI and KAERI. And JAERI-KAERI joint seminar has been held every three years. The 1st and 2nd JAERI-KAERI Joint Seminars were held in November 1992 at JAERI and in September 1995 at KAERI, respectively. The 3rd JAERI-KAERI Joint Seminar was held on 25 and 26 March, 1999 at the Oarai Research Establishment of JAERI. In this seminar, total participants of 84 were joined from JAERI, KAERI, Hanyang University, Japan Nuclear Cycle Development Institute, Oarai Branch of Institute for Materials Research (IMR) of Tohoku University, Nippon Nuclear Fuel Development Co., Ltd., Nuclear Development Corporation and others. Contributed presentations were 33 in three sessions; Current status and future perspectives on PIE (8 presentations), PIE techniques (11 presentations) and Evaluation of PIE data (14 presentations). Re-assembling technique for JOYO fuel, Nd-YAG laser welding technique, grain boundary analysis using FEG-TEM, lift time estimation of PWR Rod Cluster Control Assembly (RCCA) rodlet and failure analysis of Korea Nuclear Power Plant (KNP) fuel have been widely noticed as topic items on PIE. JAERI-Conf 99-009

And some comments from PIE user, were pointed out that the nano-PIE technique, the flexibility to ad-hoc demands on testing space or utilization, and the international collaboration were very important for the next generation's PIE

Keywords; PIE, Hot Laboratory, Re-assembling, JMTR, JOYO, HANARO, PWR, RCCA, Nd-YAG Laser, Failure Analysis, International Collaboration JAERI-Conf 99-009

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Foreword

It has been periodically carried out to bring together specialists and scientists in the field of the PIE activities and to strengthen the research cooperation between Japan Atomic Energy Research Institute (JAERI) and Korea Atomic Energy Research Institute (KAERI) through the mutual exchange of technical information on several kinds of items of Nuclear safety and Other related fields, under the Arrangement of the Implementation of Cooperative Research Program in the Field of Peaceful Uses of Nuclear between JAERI and KAERI since 1985. Between the Department of JMTR of the JAERI and the Nuclear Fuel Cycle Research Group of the KAERI, the 1st and 2nd JAERI-KAERI Joint Seminars on the PIE technology were organized by JAERI in November 1992 and KAERI in September 1995, respectively to summarize the results of mutual information exchange on the PIE activity. The 3rd JAERI-KAERI Joint Seminar was held in the HTTR main conference room at the Oarai Research Establishment of JAERI from March 25th to 26th, 1999 under the auspices of the Oarai Research Establishment of JAERI, the 2nd Seminar and three years later for summarizing the results of mutual information exchange on the PIE activity. The PIE-related persons including PIE users in and out the KAERI and JAERI took part in this seminar who belong to Hanyang University, Japan Nuclear Cycle Development Institute (JNC), Oarai Branch of Institute for Materials Research (IMR) of Tohoku University, Nippon Nuclear Fuel Development Co., Ltd. (NFD), Nuclear Development Corporation (NDC) and others. They discussed on recent topics on PIE and specially, Japanese PIE activities were briefly reviewed in this seminar by the result of participation of the JNC Oarai as a user on JMTR of JAERI. Contributed presentations of 33 were carried out in three sessions; Current status and future perspectives on PIE (8 presentations), PIE techniques (11 presentations) and Evaluation of PIE data (14 presentations) with total number of participants of 84 in two days. At the seminar, it was confirmed that key issues were to continue the mutual information change and the international collaboration and furthermore to grasp the perspectives of next generation's PIE. All the participants made an agreement to meet again in the next seminar three years later in Korea when the world-cup game on soccer will be held under the joint auspices of Japan and Korea.

JAERI-Conf 99-009

Contents

Opening Address Toshio Fujishiro 1 Key-Soon Lee 2

Session 1: Current Status and Future Perspectives on PIE 3

1.1 Over View of Nuclear Fuel Cycle Examination Facility at KAERI 5 Key-Soon Lee, Eun-Ga Kim, Kih-Soo Joe, Kil-Jeong Kim, Ki-Hong Kim and Duk-Ki Min (KAERI) 1.2 Activities on PIE of Nuclear Power Plant Fuels in KAERI 13 Eun-Ka Kim, Yong-Bum Chun, Gil-Sung You, Dae-Seo Koo, Duck-Kee Min, Key-Soon Lee and Seung-Gy Ro (KAERI) 1.3 Present Status of PIEs in the Department of Hot Laboratories 20 Tsuneo Kodaira, Tomohide Sukegawa, Hidetoshi Amano, Fumio Kanaizuka and Kiyomi Sonobe (JAERI) 1.4 Current Status and Future Prospects of JMTR Hot Laboratory 32 Osamu Baba, Norikazu Ooka and Taiji Hoshiya (JAERI) 1.5 Over View of Post-irradiation Examination Facilities for Fuels and Materials Development of Fast Reactor 44 Masahiko Itoh (JNC) 1.6(a) Activities of Oarai Branch IMR of Tohoku University as an Open Facility for Utilizing JMTR 53 Minoru Narui, Tsutomu Sagawa and Tatsuo Shikama (Tohoku Univ.) 1.6(b) Ventilation System of Actinides Handling Facility in Oarai-Branch of Tohoku University 66 Yoshimitsu Suzuki, Makoto Watanabe, Mituo Hara, Tatsuo Shikama, Hideo Kayano and Toshiaki Mitsugashira (Tohoku Univ.) 1.7 PIE Activities in NFD Hot Laboratory 75 Norikatsu Yokota, Keizo Ogata and Noriyuki Sakaguchi (NFD) 1.8 Current Status of NDC Fuel Hot Laboratory 89 Youichirou Yamaguchi, Takanori Matsuoka, Satoshi Shiraishi and Mitsuteru Sugano (NDC)

vii JAERI-Conf 99-009

Session 2: PIE Techniques 101

2.1 Development and Application of PIE Apparatuses for High-burnup LWR Fuels 103 Katsuya Harada, Naoaki Mita, Yasuharu Nishino and Hidetoshi Amano (JAERI) 2.2 A Technique of Melting Temperature Measurement and its Application for Irradiated High-burnup MOX Fuels 112 Takashi Namekawa and Takashi Hirosawa (JNC) 2.3 Development of PIE Techniques for Irradiated LWR Pressure Vessel Steels 119 Masahiro Nishi, Minoru Kizaki and Tomohide Sukegawa (JAERI) 2.4 High Resolution Grain Boundary Analysis of Neutron Irradiated Stainless Steel Using FEG-TEM 131 Mitsuhiro Kodama, Yoshihide Ishiyama and Norikatsu Yokota (NFD) 2.5 The Development of Crack Measurement System Using the Direct Current Potential Drop Method for Use in the Hot Cell —- - - 140 Do-Sik Kim, Sang-Bok Ahn, Key-Soon Lee, Yong-Suk Kim and Sang-Chul Kwon (KAERI) 2.6 Development of a Remote Controlled Small Punch Testing Machine for Nuclear Fusion Research 151 Masao Ohmi, Junichi Saito, Toshimitsu Ishii, Taiji Hoshiya and Shiro Jitsukawa (JAERI) 2.7 Newly Developed Non-destructive Testing Method for Evaluation of Irradiation Brittleness of Structural Materials Using Ultrasonic 163 Toshimitsu Ishii, Norikazu Ooka, Yoshiaki Kato, Junichi Saito, Taiji Hoshiya (JAERI), Saburo Shibata (IHI) and Hideo Kobayashi (Tokyo Institute of Technology) 2.8 Reassembling Technique for Irradiation Vehicle at Fuel Monitoring Facility (FMF) 173 Koji Maeda, Tsuyoshi Nagamine, Yasuo Nakamura, Takeshi Mitsugi and Shinichiro Matsumoto (JNC) 2.9 The Development of Electric Discharge Machine for Hot Cell Usages - 188 Wan-Ho Oh, Sang-Bok Ahn, Sang-Chul Kwon, Yong-Suk Kim and Key-Soon Lee (KAERI) 2.10 Development of Remote Laser Welding Technology 200 Soo-Sung Kim, Woong-Ki Kim, Jung-Won Lee, Myung-Seung Yang and Hyun-Soo Park (Yong-Sun Choo) (KAERI) 2.11 SEM Modification and Shielded Glove Box Design for the Radioactive Material 210 Ki-Seog Seo, Jeong-Hoe Ku, Kyoung-Sik Bang, Ju-Chan Lee, Gil-Sung You, Dae-Seo Ku and Duck-Kee Min (Dae-Seo Koo) (KAERI) JAERI-Conf 99-009

Session 3: Evaluation of PIE Data — - 217

3.1 Detection of Defects in Control Rods by Eddy Current Examination —- 219 Dae-Seo Koo, Jeong-Hoe Ku, Duck-Kee Min, Ro Seung-Gy, Young-Sang Joo and Yoon-Kyu Park (KAERI) 3.2 Life Time Estimation for Irradiation Assisted Mechanical Cracking of PWR RCCA Rodlets -- - -— 227 Takanori Matsuoka and Youichirou Yamaguchi (NDC) 3.3 Surveillance Tests for Light-water Cooled Nuclear Power Reactor Vessels in IMEF 245 Yong-Sun Choo, Sang-Bok Ahn, Dae-Gyu Park, Yang-Hong Jung, Byung-Ok Yoo, Wan-Ho Oh, Seung-Je Baik, Dae-Seo Koo and Key-Soon Lee (KAERI) 3.4 The Fracture Toughness Testing of Unirradiated and Irradiated Zr-2.5Nb CANDU Pressure Tube - - 255 Sang-Bok Ahn, Do-Sik Kim, Dae-Seo Koo, Sang-Chul Kwon and Yong-Suk Kim (KAERI) 3.5 Post-Irradiation Examination of PWR Fuels in KOREA - 267 Young-Bum Chun, Gil-Sung You, Dae-Seo Koo, Eun-Ka Kim,Duck-Kee Min and Seung-Gy Ro (KAERI) 3.6 Hydriding Failure Analysis Based on PIE Data - 278 Yong-Soo Kim (Hanyang Univ.), Hyun-Taek Park, Hwee-Soo Jun(Korea Electric Power Corp.), Yong-Bum Chun, Gil-Sung You, Duck-Kee Min,Eun-Ka Kim and Seung-Gy Ro (KAERI) 3.7 Re-Irradiation Tests of Spent Fuel at JMTR by means of Re-Instrumentation Technique - 286 Jinichi Nakamura, Michio Shimizu, Yasuichi Endo, Hideaki Nabeya, Kenichi Ichise, Junichi Saito, Kunio Oshima and Hiroshi Uetsuka (JAERI) 3.8 HANARO Fuel Gamma Scanning - - - 300 Kwon-Pyo Hong, Tae-Yon Kim, Dae-Gyu Park, Dae-Seo Koo and Bong-Goo Kim (Key-Soon Lee) (KAERI) 3.9 Metallurgical Properties of Power Reactor Fuels after Irradiation — 310 Gil-Sung You, Hang-Suk Seo, Sung-Ho Eom, Duck-Kee Min, Eun-Ka Kim, Dae-Seo Koo and Jun-Sik Ju (KAERI) 3.10 Post Irradiation Examinations for IASCC Study at JAERI - 325 Takashi Tsukada, Yukio Miwa, Hirokazu Tsuji and Hajime Nakajima (JAERI) 3.11 Determination of Irradiation Temperature Using SiC Temperature Monitors 335 Tadashi Maruyama and Shoji Onose (JNC)

IX JAERI-Conf 99-009

3.12 R&D Status and Requirements for PIE in the Fields of the HTGR Fuel and the Innovative Basic Research on High-temperature Engineering — 341 Kazuhiro Sawa, Masahiro Ishihara, Tsutomu Tobita, Junya Sumita, Kimio Hayashi, Taiji Hoshiya, Hajime Sekino and Etsurou Ooeda (JAERI) 3.13 Advanced Post Irradiation Examination for Fusion Reactor Development in JMTR 362 Kunihiko Tsuchiya, Etsuo Ishitsuka, Minoru Uda, Junichi Saito and Hiroshi Kawamura (JAERI) 3.14 Hot Cell Works and Related Irradiation Tests in Fission Reactor for Development of New Materials for Nuclear Application 373 Tatsuo Shikama (Tohoku Univ.)

Summarizing Talk Norikazu Ooka 380 Closing Address Key-Soon Lee 381 Osamu Baba 382

Appendix A Committee 383 Appendix B Schedule 385 Appendix C Program 386 JAERI-Conf 99-009

Key-Soon Lee 2

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xii JAERI-Conf 99-009

3.5 SISKfcttS PWRmM(DmmM%& - - 267 Young-Bum Chun, Gil-Sung You, Dae-Seo Koo, Eun-Ka Kim, Duck-Kee Min and Seung-Gy Ro (KAERI) 3.6 PIE x-*£«fc5#IlSffc8fcSl##f - 278 Yong-Soo Kim(Hanyang Univ.), Hyun-Taek Park, Hwee-Soo Jun (Korea Electric Power Corp.) Yong-Bum Chun, Gil-Sang You, Duck-Kee Min, Eun-Ka Kim and Seung-Gy Ro (KAERI) 3.7 teffl&$$fiffgftffi£fflufc JMTR iz&n&mmmtm -- 286 n%, ±m % mm 3.8 HANARO i^0^>YX + A'->y - - 300 Kwon-Pyo Hong, Tae-Yon Kim, Dae-Gyu Park, Dae-Seo Koo and Bong-Goo Kim (Key-Soon Lee) (KAERI) 3.9 mtspmn

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XIII JAERI-Conf 99-009

Opening Address by Toshio Fujishiro Chairman of Organizing Committee Director General, Oarai Research Establishment, JAERI

Good morning ladies and gentlemen! It is a great pleasure for us to open "The Third JAERI-KAERI Joint Seminar on Post-Irradiation Examination Technology" here in Oarai Establishment of JAERI. As you may know, this Joint Seminar is held as one of the cooperative programs on PIE techniques based on the arrangement for implementation of "Cooperative Research Program between JAERI and KAERI" The 1st seminar was held in 1992 in JAERI and 2nd in 1995 in KAERI. Through these 2 seminars as well as other activities like the exchange of experts, we have successfully continued effective information exchange on operation and management of PIE facilities, and developments of PIE technique. We now largely depend on nuclear as one of the major energy resources for electricity both in Japan and Korea. Irradiation research of nuclear fuel and materials are vital for safe and economical of the current LWR plants and also for security of future energy source including the development of future fission and fusion reactors. PIE technology should be the most important technology to support this irradiation research. In this seminar, we have about 60 participants from KAERI, Hangyang University, Japan Nuclear Cycle Development Institute, Nuclear Develop Corporation, Nippon Nuclear Fuel Development Co., Ltd. and JAERI. 33 presentation are going to be presented during the full 2 days program. We expect that this 3rd Seminar will provide a good opportunity to exchange information and to establish good personal relationship for future cooperation. I hope active discussions will be made among the participants and this seminar will be successful. Thank you.

- 1 - JAERI-Conf 99-009

Opening Address

by Key-Soon Lee Director, Nuclear Fuel Cycle Examination Team Korea Atomic Energy Research Institute

It is my great pleasure to have an opportunity to make an opening remarks for the 3rd KAERI-JAERI Joint Seminar on PIE technology being held this Oarai. First of all, I would like to express my sincere appreciation to Dr. Fujishiro, general director of Oarai Establishment JAERI, for his help on the joint seminar, and also I express my appreciation to Dr. Baba and Mr. Hoshiya and their staffs members for their efforts in organizing this joint seminar on the technology. We, both of Korean and Japanese scientists, are now preparing for the coming 21st Century. In this coming century, due to the lack of fossil resource in Korea and Japan, nuclear energy could be expected to be an unique energy source for the solution of the lack of energy resources in this two countries, as we understand the nuclear power is an economical and technology self-reliant energy source. Therefore PIE technology will be more important than ever which is essential to the development of nuclear technology to be needed for the safe utilization of the nuclear energy. At the time of the 1st seminar held at Oarai and 2nd seminar at the Daeduk Science Town, we had exchanged a lot of technical information and experiences on the PIE technologies. It is my sincere desire that this seminar also will contribute greatly to the utilization of PIE facility through exchanging of broad technical information, new ideas, and relevant experiences of PIE technology as we did at the previous seminars. As a representative of our participants from Korea, I would like to express that it is our great pleasure to be here for participation in this seminar and to share our friendship with all of you, and again I want to express my appreciation to staff members for preparation of this seminar. I hope this seminar could be remembered to be a useful seminar to all of us. Thank you very much.

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SESSION 1

CURRENT STATUS AND FUTURE

PERSPECTIVES ON PIE

PIE ACTIVITY-1 CHAIRS : N. Ooka (JAERI) and K.-S. Lee (KAERI)

PIE ACTIVITY-2 CHAIRS : E.-K. Kim (KAERI) and T. Kodaira (JAERI)

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1.1 Over View of Nuclear Fuel Cycle Examination Facility at KAERI

Key-Soon Lee, Eun-Ga Kim, Kih-Soo Joe, Kil-Jeong Kim, Ki-Hong Kim and Duk-Ki Min

Korea Atomic Energy Research Institute Yuseong-Ku, Taejon, Korea

ABSTRACT

Nuclear fuel cycle examination facilities at the Korea Atomic Energy Research Institute(KAERI) consist of two post-irradiation examination facilities(IMEF & PIEF), one chemistry research facility(CRF), one radiowaste treatment facilty(RWTF) and one radioactive waste form examination facility(RWEF). This paper presents the outline of the nuclear fuel cycle examination facilities in KAERI.

INTRODUCTION

The research and operation team for nuclear fuel cycle examination of Korea Atomic Energy Research Institute(KAERI) was organized in order to promote the operation efficiency of nuclear fuel cycle examination facilities. The team is responsible for operation of five examination facilities i.e., two facilities for post- irradiation examination of nuclear fuel and materials, one chemistry research facility, one facility for the treatment of low level radiowaste and one facility for safety tests of radioactive waste. The number of persons worked in five facilities is 59 persons and operation budget is about four billion Won(3.3 million US$). This paper introduces outline of the nuclear fuel cycle examination facilities operated by the team.

GENERAL DESCRIPTION OF EACH FACILITY

1. Post-Irradiation Examination Facility (PIEF)

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Kori Unit 1, which was the first nuclear power reactor in Korea, was commercially operated in 1979. So the post-irradiation examination of spent fuel and structure discharged from this reactor was necessary in order to probe the reliability of nuclear fuel and structure material. In response to such approval, the KAERI decided to construct the PIEF for examination of spent fuel and structural material of power reactor. The PIEF started to design and construct in 1980 and completed at the end of 1985. The qualification of the equipments and test operation of the facility was conducted before 1987, and the PIEF has been put into service since 1987. A full size spent fuel discharged from commercial PWR could be subjected to post irradiation examination at this facility. The facility provides adequate services of examination for spent fuel as well as for examination associated with reactor safety, and fuel fabrication technology improvements. The PIEF is a two-story building with a basement. A total floor area of the building is about 5,947 m2 The PIEF has three large pools(9401 -9403), four concrete cells(9405 - 9407) and two lead cells(9408 and 9409). Specifications and detail examination items of the pool and hotcell in the PIEF are summarized in Table 1.

2. Irradiated Material Examination Facilities (IMEF) IMEF was constructed by domestic technology in order to mainly conduct post- irradiation examination of fuel and material irradiated in HANARO(High Flux Advanced Neutron Application Reactor), which provides high neutron flux levels among research reactor in the world. The facility commenced to design and construct in 1988 and completed at the end of 1993. The qualification of the equipments and test operation of the facility had been conducted by the end of 1994 and the IMEF has been put into service since 1995. The facility has three stories and a basement with a total floor area of about 4,000m2, and concrete cells of about 60m in total length. The facility consists of fuel examination cell line, material examination cell line and multiple examination cell line, and has 26 work units(one unit has one window and one pair manipulators) The activities conducted in the fuel examination cell line are a dismantling of capsules and fuel bundle, visual inspections, X-ray radiography, dimensional measurements, gamma scanning and eddy current tests for nondestructive test, and fission gas collections and sample preparation for metallography for destructive test, and the activities in the material examination cell line are the measurement of mechanical and physical properties of irradiated material, impact test, tensile test, heat treatment, and thermal conductivity measurement. A lead cell is also available for metallography, hardness test, and density measurement. - 6 - JAERI-Conf 99-009

The multiple examination cell line is used for the special research handling irradiated fuel and material. This cell line will be used for technology development of fuel fabrication using of PWR spent fuel a special project of Direct Use of PWR spent fuel in CANDU (DUPIC) research. In addition, a shielded electron probe microanalyzer and a transmission electron microscope installed in hot room are used in the examination of irradiated fuel and material. The specifications and detailed examination items carried out in the IMEF are summarized in Table 2.

3. Chemistry Research Facility (CRF) Chemistry Research Facility started to design in 1989 and constructed at the end of 1992. The facility has four stories with total floor area of about 3,300 m2. Major facilities of CRF consisted of 24 cold laboratory including clean laboratory, low level radioactivity measurement laboratory, and one radiochemical laboratory including one set of lead shielded line having three compartments with lead glass windows, two sets of steel boxes, four set of glove boxes and two liquid waste storage tanks capable of 10 cubic meters in capacity. In this facility 43 analytical instruments such as thermo-ionization massspectrometry(TI-MS), ICP-AES with shielded and non-shielded equipment, emission spectrograph, a,/3 ,y- measurement system, quadrupole mass spectrometer, EPMA, hydrogen determinator, XRD, XRF, XPS/Auger/SMS and ICP-MS etc. were installed and put into services of chemical analysis for the research and other works. A major activity of CRF is to do chemical analysis of irradiated samples for the post-irradiation examination such as burnup measurement and non-radioactive samples from the research projects such as fuel development and reactor material development. The lead shielded line is used for dissolution of irradiated fuel. A burnup measurement is performed by chemical analysis of irradiated fuel after dissolution, dilution, separation and determination of burnup monitors of uranium, plutonium and Neodymium using chemical hot cell, glove box and other analytical instruments. In addition, fission product determination, fission gas determination, hydrogen determination in zircaloy tube and some elemental analyses are also performed in this facility. Two liquid waste storage tanks are used for receiving non-radioactive waste solution and radioactive waste solution in each. The received wastes are transferred to Radioactive Waste Treatment Facility for the waste treatment.

4. Radioactive Waste Treatment Facility

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The radwaste treatment facility(RWTF) was designed and constructed by the domestic technology on the basis of the conceptual design from France. The RWTF has been normally operated since March, 1991 under the license by Korea Institute of Nuclear Safety(KINS). Major waste treatment process consists of liquid waste evaporation, bituminization, solar evaporation and solid waste compaction system. Figure 1 shows the radioactive waste treatment process flow diagram of the RWTF. The low-level waste(5X 10"6 fid/ml < LAW < 1 juCi/ro£) is usually treated by the evaporation process. The evaporator is the forced circulation, long-tube vertical type having high heat coefficients and its evaporation capacity is 1.2 m3/hr. For the bituminization process, the thin film evaporator is installed and its evaporation capacity is 40 I /hr at 240 °C. The straight asphalt 60/70 is used as a matrix agent for the process. The solar evaporation facility was designed and constructed by KAERI's own technology based on the Zero Release Concept for the very low-level liquid radioactive wastes(VLAW). The annual treatment capacity of the solar evaporation facility is 1,200 m3. The VLAW and the condensate from evaporation below the concentration of 5 X 10"6 y. Ci/m£ are treated in the solar evaporation facility. All of the radioactive wastes generated from the post irradiation examination facility(PIEF) and the laboratories in KAERI have been treated in the RWTF, whose major radionuclides are Co-60 and Cs-137. The generated wastes such as very low- active liquid waste(VLAW), low-active liquid waste (LAW), and medium-active liquid waste(MAW) from PIEF are transferred to the RWTF through the pipe line. Spent resin is also transferred by the pipe line. While corrosive active liquid waste(CAW) is transported by the specially designed tank-car. Recently, the radioactive wastes from the research reactor, HANARO, has begun to be generated. The HANARO has been operated since April, 1995. There are three major buildings; the reactor building, the radioactive isotopes production facility(RIPF), and the irradiation material examination facility(IMEF). The radioactive waste from those buildings are collected and transferred to the RWTF through the pipe line depending on the radioactivity level. The maximum volume of the waste treated is estimated to be 240m3/yr for the VLAW, 230m3/yr for the LAW, and 6m3/yr for the MAW. Approximately, 82% of the VLAW and 87% of the LAW at HANARO are generated from the RIPF building. In case of the RIPF building, 88% of the VLAW is the handwashed waste, and 97% of the LAW is from the hot sink, fume hood, and glove box.

5. Radwaste Form Examination Facility (RWEF)

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Radwaste Form Examination Facility was constructed to establish waste acceptance criteria for disposal site, and now carry out a characterization of waste form to provide technical data for feedback to solidification process(KAERI, KEPCO's NPPs) and for establishment of national regulation. This facility has two stories( 1,350 m2) and was completed to construct in the middle of 1992 through a national inspection of the equipments and installations. The characteristics(radioactivity, mechanical and physicochemical properties) of waste forms against radionuclides release are important. Principal examination items are radionuclides assay in 100~200drum by non-destructive method, compressive strength, long/short-term leach test(including 200drum), thermal cycling test, free liquid test, etc. Core drilling machine and core specimens sizing machine are used for lab. scale examination from real drum(rigid and flexible solidification matrix). These test are carried out remotely in concrete shielded cell. In addition, this facility being capable of handling high activity will be assist and support IMEF and other R&D studies, this year.

OPERATION STAFF AND BUDGET

Total number of operation staffs are 52 persons and the operational budget of the Nuclear Fuel Cycle Examination Facility is about four billion won (3.3 million US$) and more detailed information is presented in Table 3.

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Table 1 Specifications and fuctions of pool and hotcell in PIEF

Inside Wall Number Pool Dimension Thickness of Functions Major Cell Equipment /Cell WxDxH(m) (cm) Windows

Normal 9401 6.5 x 3.0 x Concrete Unloading /Pooll 15.5(D) 110

Normal 9402 6.5 x 3.0 x Concrete Storage /Pool 10.0(D) 110 Visual Inspection, Video Camera Normal 9403 7.5 x 3.0 x Eddy Current Test, Eddy Current Tester Concrete 1 /Pool 15.5(D) Dimensional Measurement, Gamma Scanning Equipment 110 Axial Gamma Scanning Saw Visual Inspection, Porfilometer, Heavy Eddy Current Test, 9404 6.5X1.5X3.5 Concrete 3 Dimensional Measurement, Eddy Current Tester /Cell 85 Axial Gamma Scanning Gamma Scaning Equipment. X-ray Radiography X-ray Equipment Heavy Rod Cutting Rod Cutter 9405 4.0X1.5X3.5 Concrete 2 FP Gas Collection Rod Puncturing Apparatus /Cell 85

Heavy Specimen Storage Storage Rack 9406 2.0X1.5X3.5 Concrete 1 Specimen Identification /Cell 85

Heavy Specimen Preparation Micro Cuter, Mounting Press 9407 3.0X1.5X3.5 Concrete 2 for Metallography Grinder/Polisher, Periscope /Cell 85 Specomen Preparation of SEM Metallography Microscope, 9408 Lead 1.2X1.8X2.5 2 Micro Hardness Tester /Cell 0.2 Hardness Measurement Macrosope Sectional Gamma Scanning Micro Gamma Scaning 9409 Lead 1.2X1.8X2.5 1 Equipment. /Cell 0.2 Density Measurements Balance

-10- JAERI-Conf 99-009

Table 2 Specifications and functions of hotcell in IMEF

Inside Wall Number Major Cell Cell Dimension Thickness of Functions Equipment W X D X H(m) (m) Windows

Visual inspection, Porfilometer, Eddy current test, Dimensional Eddy Current Tester Heavy measurement, Ml 7.0X3.0X6.0 Concrete 3 Axial gamma scanning Gamma Scaning Cell 1.2 Equipment. X-ray radiography X-ray Equipment FP gas collection Rod Puncturing Apparatus Dismantling of capsule Milling Machine, Heavy and fuel bundle Rod Cutter M2 7.0X3.0X6.0 Concrete 3 Preparation of Electric Discharge Cell 1.2 Mechanical test Machine specimen Preparation of Micro Cuter, Heavy metallography sample Mounting Press M3 4.7X3.0X6.0 Concrete 2 Preparation of EPMA Grinder/Polisher, Cell 1.2 sample Periscope

Specimen storage Storage Rack Heavy M4 Specimen 2.3X3.0X3.0 Concrete 1 Cell identification 1.2 Charpy impact test Impact Tester, Heavy M5a Heat treatment Heating Furnace 7.1X2.0X4.0 Concrete 3 Cell Physical properties Thermal Diffusivity 0.8 measurements Tester, Dilatometer

Tensile/compression Dynamic Tensile Heavy test Tester M5b 4.8X2.0X4.0 Concrete 2 Fatigue test Static Tensile Cell 0.8 Tester, High Scope M6a Heavy Pellet manufacturing Pellet 11.7X2.0X4.0 5 Cell Concrete manufacturing Heavy Rod and bundle Rod and bundle M6b 11.7X2.0X4.0 Concrete 5 manufacturing manufacturing units Cell 1.1 Metallography Microscope, M7 Density measurements Micro Hardness 1.5X2.6X2.65 Lead 0.2 2 Cell Tester Balance

- 11 - JAERI-Conf 99-009

Table 3 The Number of persons and operation budget of fuel cycle examination facilities of KAERI in 1998

KEARI Staff Post Doctor Others Budget (million US$) PEEF 12 1 0.94 IMEF 14 2 2 0.79 CRF 10 1 0.67 RWTF 12 1 0.65 RWEF 4 0.26

Fig. 1 Flow Diagram of Radioactive Waste Treatment Process

-12- JAERI-Conf 99-009 JP9950623

1.2 ACTIVITIES ON PIE OF NUCLEAR POWER PLANT FUELS IN KAERI

Eun-Ka Kim, Yong-Bum Chun, Gil-Sung You, Dae-Seo Koo, Duck-Kee Min, Key-Soon Lee, Seung-Gy Ro

ABSTRACT

The PWR irradiated fuels were transported from NPPs pool sites to KAERI PIE facility by using a shipping cask. Post-irradiation examination of reactor fuels has been performed to evaluate the performance and integrity in pools and hot cells since 1987. In this paper, 10 years of PIE activities for the power reactor fuels conducted at PIE facility in KAERI were summarized with a brief description of PIE capabilities.

INTRODUCTION

The nuclear power plant (NPP) in Korea went into commercial operation in 1978. Today total eleven(ll) PWRs and three CANDU NPPs are in operation. From the early of 1980's indigenous nuclear fuel development program has been started. Subsequently, post-irradiation examination (PIE) facility for the nuclear fuels was indispensable to make sure of the integrity and irradiation performance of these fuels. Construction of the PIE facility was completed at the end of 1985. After one year test operation of the facility, it has been put into service for PWR fuels from 1987.

TRANSPORTATION OF IRRADIATED PWR FUELS

The irradiated fuel assemblies have been transported from PWR nuclear power plant (NPP) pool sites to the KAERI PIE facility by using a shipping cask (KSC-1) which was designed for the transportation of one spent PWR fuel assembly. Seven spent PWR fuel assemblies and one basket containing the 46 defective fuel rods were transported for PIE by 1993. Two defective PWR fuel rods from Yongkwang Unit 4 and three defective PWR fuel rods from Ulchin Unit 2 were transported in 1996 and in 1998, respectively. Table 1 shows the status of PWR fuels transported to PIE facility in KAERI.

-13- JAERI-Conf 99-009

POOL EXAMINATION PROCEDURE

Fig. 1 shows the layout of ground floor plan of the PIE facility in KAERI. The shipping cask trailer comes in the receiving area through the shipping cask receiving entrance (6421) and the cask is transferred from trailer to decontamination pit by a 50 tone overhead crane. The cask is put upright at center of the room and the cask surface is washed with high-pressurized water spray. And then the cask is connected to the circulation loop for internal decontamination. With this close circuit processing device, cask is cooled down to mitigate the thermal shock when the fuel is loaded in the pool and the pressure and contamination level of radioactivity built up in cask are lowered. After decontaminating the cask, it is transferred to the pool 9401 for unloading of fuel assembly. Then, the fuel assembly is transferred to the storage pool 9402 for a temporary storage before inspection in the next pool. In the third pool, fuel inspection and dismantling are carried out. Before dismantling, the fuel assembly is inspected with the visual and dimensional inspection system (VDIS) by checking the geometrical changes, dimensions, and visual conditions. After finishing these examinations, the top nozzle of the fuel assembly is removed to extract the fuel rods to be examined in hot cell. The extracted fuel rods are transferred one by one to the hot cell 9404 using the lifting cart system.

HOT CELL EXAMINATION

The fuel rod transferred from the pool 9403 is placed on the rod examination bench for subsequent nondestructive test, which is vertically positioned in the NDT cell 9404. The nondestructive test of fuel rod is performed starting with visual inspection and photography, profilometry, eddy current test, X-ray radiography, and axial gamma scanning, etc. After nondestructive examination, the rod is tilted to the horizontal position and then transferred to the next cell, rod cutting cell 9405. Fission gas sampling is made by a puncturing device incorporated with a system outside the cell 9405 and the samples are sent to the analytical laboratory for chemical composition analysis. Cutting and drilling of the fuel rod are carried out in the cell 9405. Usually the PWR fuel rod is cut as long as 60cm, and six or seven samples of 2cm in length are taken from each rod. The 60cm long sections which are not examined are put in a container, and then transferred to the pool 9402 for a storage. For metallographic sample preparation, sectioning, resin impregnation, mounting, grinding, polishing, and chemical etching are performed in the sample preparation cell

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9407. Optical macro- and microscopic examination and photography are performed in the lead cell 9408. Sectional or radial gamma scanning and density measurement of fuel samples are carried out in the lead cell 9409. The burn-up is determined by Nd isotope ratio which is chemically separated from the irradiated fuel samples at cell 7409. Physical and mechanical tests for irradiated fuel materials are performed in the irradiated material examination facility (IMEF) located near PIE facility.

PIE OF IRRADIATED PWR FUELS

Post-irradiation examination for the discharged and failed PWR fuels has been performed at PIE facility in KAERI. As shown in table 2, irradiated PWR fuels took a series of pool examinations for fuel assembly, hot cell nondestructive examinations of fuel rods and destructive examinations of fuels in hot cells (1-4). PWR Fuel assemblies are examined on visual inspection, dimensional measurement, and burn-up distribution measurement by gamma scanning. Hot cell nondestructive examination includes visual examination and photography, profilometry, eddy current test, X-ray radiography, axial gamma scanning, and oxide layer thickness measurement. Destructive examination of fuel rods covers fission gas sampling and analysis, burn-up measurement, density measurement, metallography, and sectional gamma scanning.

SUMMARY

The performance and integrity test of the irradiated PWR fuels have been conducted at PIE facility in KAERI since 1997. The spent PWR fuels are continuously examined in KAERI PIE facility as one assembly per annum. Recent concentrations of PIE items are put on the enhancement of the irradiation characteristics of fuels to endure under more severe conditions and environment in consideration of high burn-up. PIE database for supporting safe operation of NPPs and improvements of fuel performances are under construction by using the data obtained through PIE so far.

REFERENCES

1. S.G. Ro et al., "Post-Irradiation Examination of Kori-Fuel" KAERI/GP-77/88 (1988).

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2. E.K. Kim et al., "Hot Cell Examination of Kori-3 Defective Control Rod" KAERI/TR-141/89(1989).

3. S.K. Lee et al., "Confirmation of Failure Causes of the Kori-2 Cycles 7&8 KOFA Fuel and Remedies against the Fuel Failure" KAERI/TR-387/93 (1993).

4. S.G. Ro et al., "Post-Irradiation Examination of Yongkwang-4 Defective Fuel rods" KAERI/TR-739/96 (1996).

-16- j 74W LEPMALab 7430 Low Active 7411 ialfon Radwaste tamrina L* 3.

Aniilysis Chemical Hol-Cdl SMctromttr] Lab. I ftutr. Decon. $421 Cask Receivtng Area htcasuriae 8401 Lab. Intervention Act* 7410 Atomic Spectroscope Lab.

6405 O Safety O Control

General Chwnbtey Lab.

Changing Room

Fig. 1. Layout of Ground Floor Plan of the PIEF JAERI-Conf 99-009

Table 1. Transportation of PWR Fuels Irradiated in NPPs

Fuel Assy. Date of Date of NPP FA No. Status Type Discharged Transported

Kori Unit 1 C15 14x14 17 Apr.'82 April, 1987 Intact

5) A39 55 30 Jan.'81 May, 1987 Intact

55 A17 55 27 Oct. '79 June, 1987 Intact

55 Basket (46 Rods) 55 May, 1988 Defect

55 G23 5? 24 Oct. '86 May, 1990 Intact

55 J14 55 20 Jan.'89 July, 1991 Intact

5) F02 55 17 Sep.'85 May, 1992 Intact

Kori Unit 2 J44 16x16 29 May '92 April, 1993 Defect Yongkwang B209-R8 (Rod) 16x16 24 Sep.'95 April, 1996 Defect Unit 4 55 D108-K2 (Rod) 55 55 April, 1996 Defect Ulchin Unit 2 J09-L1 (Rod) 17x17 12 May '97 July, 1998 Defect

55 J09-K1 (Rod) 5) July, 1998 Intact

55 J12-A13 (Rod) July, 1998 Defect

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Table 2. PIE of Irradiated PWR Fuels

Burnup Burnup FA No. Reactor Core Location PEE Status Cycle (MWD/MTU)

C15 Kori-1 1/2/3 K3/F8/H3 32,300 Dismantled

A39 53 1/2 K7/G7 25,300 5)

A17 33 1 J6 17,071 5)

Basket (46 » PIE of 4 defect rods) rods G23 4/5/6/7 A8/AS/B7/D7 35,500 Dismantled

J14 5) 7/8/9 E9/J5/H11 37,840 n NDEin F02 33 4/5/6 B6/K9/L10 28,300 Pool J44 Kori-2 7/8 C8/C7 35,018 Dismantled

B208-R8 (Rod) Yongkwang-4 1 C7 - NDT,DT

D108-K2 (Rod) 55 1 D13 - »3

J09-L1 (Rod) Ulchin-2 7 F2 11,806 33

J09-K1 (Rod) 5) 7 F2 35 NDT

J12-A13 (Rod) 5S 7 A8 7,210 NDT,DT

-19- JP9950624 JAERI-Conf 99-009

1.3 Present Status of PIEs in the Department of Hot Laboratories

Tsuneo KODAIRA, Tomohide SUKEGAWA, Hidetoshi AMANO, Fumio KANAIZUKA and Kiyomi SONOBE

Department of Hot Laboratories, Tokai Research Establishment Japan Atomic Energy Research Institute Tokai-mura, Naka-gun, Ibaraki-ken, 319-1195, Japan

ABSTRACT

The Department of Hot Laboratories (DHL) operates three hot cell facilities including the Research Hot Laboratory (RHL), the Reactor Fuel Examination Facility (RFEF) and the Waste Safety Testing Facility (WASTEF). The RHL is performing post irradiation examinations (PIEs) for fuels and materials irradiated in research and test reactors. The RFEF is principally examining the reliability of operating power reactor fuel assemblies for PWR, BWR and ATR. In the WASTEF, development and characterization tests of advanced waste forms have been carried out for a safety examination on disposal of high level waste. The present paper mainly describes current status of PIEs in these facilities and several technical topics concerning measurements of physical and mechanical properties for light water reactor (LWR) fuels and materials.

1. INTRODUCTION

DHL is operating three hot cell facilities, i.e. the RHL , the RFEF and the WASTEF. The RHL was established in 1961 and expanded in 1965 in which there are 10 /? y concrete and 38 /3 y lead cells. The RFEF was established in 1979 and it is equipped with 6 j3 y concrete cells and lay ones with 2 lead cells. The WASTEF was established in 1981 and it is equipped with 3 j3 y concrete cells, lay ones with 1 lead cell and 6 glove boxes. In this report, current activities of these facilities are described and several R & D works are also presented as technical topics.

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2. CURRENT STATUS

2.1 RHL Figure 1 shows typical PIE flow diagram in the facility, where material examination occupies relatively important position. The activities in the facility are divided into the following four categories:

Visual Inspection Dimensicn Ivfeas Irradiated Specimen X Ray Radiography at Eddy Qnot Test y-Ray Scanning Density Kfeasunexnent

N4cro-Analysis: Fuel Specimen XRay rjiffiacticn FP C3as Analysis

Visual Inspection dimension tvfeas.

Pvfeffierial Specimen Hardness Test

Tensile Test Bending Test pg "Tests oifFuel ancl Impact Test fcr Txicai ftwer St. Fatigue Test Fracture: Toughness Crack Propagation Punch

Fig.l Flow Diagram of PIEs in the RHL

(a) PIEs of HTTR Fuel Specimen The High Temperature Engineering Test Reactor (HTTR) established the first criticality on November, 1998 at the Oarai site in JAERI, where prismatic fuel compacts including coated particle are used for the driver fuel. JAERI has been studying the behavior of this type of fuel for long period and still now carry out the irradiation test using the Japan Material testing Reactor (JMTR). For PIEs of the HTTR fuel specimen, the facility has developed lots kinds of special devices such as high temperature annealing and defective fuel detecting devices, for dealing with the coated fuel particles with the size less than 1 mm in diameter.

(b) PIEs of NSRR Experimented Fuel Specimen One of the important subjects for reactor fuels is safety investigation under transient power increase. The fuel durability under the condition is examined using the Nuclear

- 21 - JAERI-Conf 99-009

Safety Research Reactor (NSRR). Specimens, prepared from the reactor fuel rods with high burnup after finished PIEs, have been supplied for reactivity initiated accident (RIA) experiment. For the specimen after the NSRR power transient test, main targets in PIE are ceramography and EPMA in the defected region.

(c) PIEs of Several Materials The facility equips several kinds of apparatus for examining mechanical properties of the materials on reactor pressure vessel, fuel cladding, first wall of fusion reactor and so on. These apparatus are mainly installed in the lead cell line in the facility, which are on tensile, impact, fatigue, fracture toughness and small punch tests.

(d) Monitoring Tests for Reactor Fuel and Pressure Vessel from JAPCO For 33 years, the facility has cooperated with the fuel monitoring works on the uranium/magnox driver fuels and the surveillance test on the reactor pressure vessel in the Tokai Atomic Power Station of the Japan Atomic Power Company (JAPCO). PIE items are visual inspection, dimensional measurement, X-ray radiography, metallography and density measurement for the fuel and Charpy impact and tensile tests for the pressure vessel. These monitoring tests have successfully finished this year due to the termination of the reactor operation.

2.2RFEFr> The RFEF is principally used for examining reactor fuels. The flow diagram on PIEs is presented in Figure 2, and the working activities in the facility can be divided into the following six categories:

Fuel Asserrtiy Fuel Rod Fuel Specimen

Visual Inspection Visual Inspection Cfexwrography Dimension Mam. r-Ray Scanning Buxnup Ivfcas. Rod GapNtas Ciiraisicn IVfcas Density IVfeas, Eddy Curoent Test Qtt-Gas Analysis Oddc Thickness IVfcas XRay Efcffincticn XRay Radiography rvfcJting Pfcint Nfeas. ¥YC Cep rvfaw Therm. ESflu. Ivfcas. FP Gas Analysis IM^, ERVIA. Punc ture Test 7 Scanning

Struztual Tvlalenul CWVting Specimen

Rod VUthdravteft Ftorce IVfcas.

Tensile Test Burst Test SCC Test t^drogn Analysis

Fig.2 Flow Diagram of PIEs in the RFEF

- 22 - JAERI-Conf 99-009

(a) PIEs of Reactor Fuels PIEs for PWR, BWR and ATR fuel assemblies are being conducted after the establishment of the facility in 1979. The developing targets of reactor fuels in Japan are aiming at higher performance and higher burnup from the standing point of economical view, so that the contents of PIEs are extended and focussed on detailed and microscopic investigations. As a series of high burnup program on PWR fuel, the fuel assembly with the burnup of about 48 GWd/tU was transferred into the facility in March 1996, and PIEs are under way.

(b) PIEs of Plutonium Fuels JAERI is investigating the irradiation behavior of uranium/plutonium mixed fuels such as (U,Pu)O2, (U,Pu)C and (U,Pu)N. Up to the present, total seven fuel specimens irradiated in the JMTR have been supplied for PIEs using the cell in the facility. For these examinations, the cells are kept in argon gas atmosphere for preventing the oxidation of specimen.

(c) Other PIEs PIEs were conducted for the two kinds of specimens. One is PIEs for the higher burnup UO2 specimens irradiated in the Halden reactor in Norway up to the burnup of about 60GWd/tU. Principal target in PIEs is in ceramography on rim structure. Another is the examination of Rock-Like fuels which are possible to dispose directly. Small fuel samples were irradiated for four cycles at the JRR-3M to clarify irradiation behavior under LWR condition. NDEs (visual inspection, X-ray photography, etc.) and DEs (puncture test, metallography, EPMA, etc.) were performed.

(d) Re-assembling of Fuel Rods Finished PIEs The fuel rods finished PIEs in the facility should be re-assembled together with the residual fuel rods and transferred to the reprocessing plant in accordance with the government policy. Re-assembling, nowadays, becomes popular work in the facility.

(e) Re-fabrication sand Re-irradiation Test JAERI is performing the reactivity experiments using the NSRR and the power ramping experiments using Boiling Water Capsule (BOCA) instrument in the JMTR, respectively. In the present, reactor fuel rods with high burnup are supplied for these experiments. Re-fabrication means the preparation of capsule for re-irradiation, and total 59 capsules, including PWR, BWR and ATR spent fuel rods with high burnup, have been re-fabricated in the facility.

(f)VEGA An experimental program, VEGA (Verification Experiments of FP Gas/Aerosol release) has been performed at JAERI to investigate the release of FP (Fission Products)

-23- JAERI-Conf 99-009 including non-volatile and short life radionuclides from irradiated fuel at -3,000 °C under high pressure condition up to 1.0 MPa. One of special features of this program is to investigate the effect of ambient pressure on the FP release from fuel that has never been examined in previous studies. In the experiment, the Japanese PWR/BWR irradiated fuels and TMI-2 debris sample will be used as the test sample. The test facility has installed into the beta/gamma concrete No.5 cell at the RFEF. Four experiments in a year will be schedule after FY 1999.

2.3 WASTEF In the WASTEF, safety examination on disposal of high level waste has been performed, as seen in Figure 3. The working activities are divided into the following five categories:

Fabrication ancl Characteristi 'WSiste Fcms

Fabrication, and CHiaracteristics of HxaninatLcns en Glass "Wfeiste Forms in Storage and disposal

Fig.3 Flow Diagram of Safety Examination in the WASTEF

(a) Fabrication of Glass Waste Forms The facility installs a glass vitrification apparatus in the concrete cell No.2, by which a glass waste forms is fabricated for examining its characteristics. High level liquid waste (HLLW) is transferred from the reprocessing plant in the former Power Reactor and Nuclear Fuel Development Corporation, PNC, (The Japan Nuclear Cycle

-24- JAERI-Conf 99-009

Development Institute, JNC, at present) to the facility. Basic characteristics, homogeneity and chemical composition are mainly evaluated by using the fabricated waste forms. This study will be terminated within this fiscal year (FY 1998).

(b) Fabrication of Synroc Waste Forms Synroc waste forms, one of the advanced materials for confining especially transuranium (TRU) elements, is under investigation. The present waste forms have relatively excellent characteristics comparing with that for glass waste forms; high density, high thermal durability and high confining performance for TRU nuclides. The cooperative study for examining the characteristics in Synroc waste forms has been undertaken between JAERI/Japan and ANSTO/Australia. This research will be finished within FY 1998.

(c) Safety Examination on Disposal The volatility of FP and TRU nuclides is one of the subjects to be studied under storage condition and the facility equips a volatility measuring apparatus. On the other hand, de-vitrification behavior in amorphous glass and alpha acceleration test on radiation damage are also carried out for the subjects under disposal condition. The most important examination under disposal condition is leachability of FP and TRU nuclides from the waste forms. The reaching test is now carried out in the reducing condition and the mobility of these nuclides in a specific rock is also examined.

(d) Technical Development on Chemical Analysis Chemical analyses occupy an important position in the facility, since the whole specimens after examinations should be subjected to the chemical analyses. The facility has several apparatuses for chemical analyses such as Induction Coupled Plasma (ICP), atomic absorption analysis and radiation spectrometers. Furthermore, technical developments on chemical analyses are continuously carried out according to further new demands.

(e) Other Tests New studies are under way concerning the corrosion test of reprocessing plant materials such as stainless steels and zirconium alloys, and the evaluation of basic characteristics on TRU nitrides such as AmN as a R&D for the advanced nuclear fuel cycle. PIEs about the irradiation assisted stress corrosion cracking (IASCC) of stainless steels for a LWR are also planning to be initiated next year.

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3. TECHNICAL TOPICS

For the evaluation of safety, reliability and integrity of LWRs, various PIEs have been carried out in the Development of Hot Laboratories concerning reactor pressure vessel steels, fuel pellets, claddings and so on. The developments of innovative and advanced apparatuses and technologies are essential in order to produce useful and high quality data in accordance with current and future PIE needs. Several technical topics are summarized as follows.

3.1 New PIE apparatuses for thermal properties measurements and microscopic analysis on LWR fuels Measurement of thermal properties and microscopic observation and analysis of irradiated fuels are very important to evaluate fuel behavior in the high burnup state. The RFEF is under development of the Pellet Thermal Capacity measurement (PTC) and Micro Density Measurement (MDM) apparatuses for the former and the Ion Microprobe mass Analyzer (IMA) and shield-type Field Emission Scanning Electron Microscope (FE-SEM) for the latter. These are outlined as follows and more details are described in the separated report2).

(a) Pellet Thermal Capacity measurement apparatus (PTC) and Micro Density Measurement apparatus (MDM) Two new apparatuses are developed to improve the accuracy of thermal conductivity of irradiated UO2. The thermal conductivity ( K ) is calculated from the following equation: K = a • Cp * p where a is the thermal diffusivity from the Pellet Thermal Diffusivity Measurement apparatus (PTDM), Cp is the thermal capacity and p is the density. The thermal capacity and the density are generally referred from previous works. Experimental data are strongly needed for the more detailed evaluation of high burnup fuel behavior. PTC based on differential scanning calorimetry and MDM based on immersed method (meta-xylene) are developing to measure the thermal capacity and density using small sample as the same as that for PTDM. Relation among PTDM, PTC and MDM is shown in Figure 4.

(b) Ion Microprobe mass Analyzer (IMA) Quantitative and qualitative analyses of micro-region in pellet and cladding are strongly needed to clarify the irradiation behavior of fuels with higher burnup in LWR. The RFEF is now under development of IMA to analyze isotope distribution on the surface as well as the depth direction. IMA consists of beam, sample, vacuum, detection control and data processing systems in the wall (200mm thickness) for radiation shielding.

26 - JAERI-Conf 99-009

The beam system has gas and Cs ion guns as a primary ion source. The gas ion gun is used for releasing positive secondary ion efficiently in order to analyze FP, TRU and so on. Minimum beam radius is less than 0.6 n m. The Cs ion gun is applied to release negative secondary ion efficiently for the analysis of oxygen within oxidation films on the cladding surface. Minimum beam radius is less than 2 n m. The sample handling system mainly consists of analysis chamber, sample entry chamber and sample stage. It is possible to evacuate in the analysis chamber beyond 4X 10~8Pa . The sample stage is possible to move in straight, rotation and tilt motions. The detection system is mounted for mass-analysis (1 to 450amu) of released secondary ions. IMA will be used for irradiated specimens in 1999.

Main body of DS C Micro-weighine machine

_ Spec imen DSC Signal Heat power suppIy

Conttroller and data process Ing unit

I 1 - ! 1 P D M 1

r i J=fellet <&• i Ther mal Property ure i in Irradated fuel i pellet measu j

Figure 4. Relation among PTDM, PTC and MDM

(c) Shield-type Field Emission Scanning Electron Microscope (FE-SEM)

The remarkable phenomena occurred in LWR fuel pellets are rim-region on UO2 pellet, hydride and zirconium oxide layer in zircaloy cladding with increasing burnup. In response to these, FE-SEM is under development with remote handling operation. FE-SEM consists of field emission gun, vacuum control and Energy Dispersive x-ray Spectroscope (EDS). The field emission gun has higher brightness than tungsten-hairpin filament type. Resolution of FE-SEM is 2nm and it will be available in 1999 for irradiated sample.

-27- JAERI-Conf 99-009

3.2 Development of mechanical testing technologies for LWR pressure vessel steels Mechanical properties of reactor pressure vessel (RPV) steels and structural materials of LWRs at the post irradiation state are the key parameter for the evaluation of safety, structural integrity and lifetime as well as the material development. The mechanical tests at the RHL have been performed for 37 years to support R&D works at JAERI. Recently, the existing Charpy impact testing machine was remodeled in order to improve its accuracy and reliability. By this remodeling, absorbed energy and other useful information can be delivered from one-time blowing. In addition, the remote machining technology from actually irradiated RPV steels has been developed in order to clarify the aging behavior of LWRs at the RHL. Another new technique is developed to determine the post-irradiation fatigue characteristics of structural and fuel cladding materials as low and high-cycle fatigue tests technology with the function as tensile test equipment. This paper outlines two mechanical testing apparatuses and techniques and remote machining of mechanical test pieces for irradiated LWR-RPV steels as follows. More details are described in the separated report3).

(a) Remodeled Charpy impact testing machine The Charpy impact testing machine was redesigned and modified in order to clarify the neutron irradiation embrittlement behavior of LWR-RPV. This machine instrumented with electronic measuring devices to detect an impact force and a displacement of specimen has an automatic specimen setting system. The block diagram of instrumented Charpy impact testing machine is shown in Figure 5.

displacement aeasuring sytten force measuring system

Figure 5. Block diagram of instrumented Charpy impact testing machine

- 28 - JAERI-Conf 99-009

The load capacity is 300J and it is possible to test in the temperature range from -140°C to 240°C by using two types of agitated liquid baths. The test specimen is transferred from the cooling (or heating) bath to an anvil of the machine using industrial robot, and struck by a hammer within 4 sec after removal it from the medium. The test items are V-notch Charpy impact test and K, d dynamic fracture toughness test. The sensor for the load detection was composed of two semiconductor active strain gages on the tup and two dummy gages put on near the hammer. Moreover, a potentiometer for the displacement detection was inserted and fixed to the hammer shaft. These signals from sensors are recorded in the wave-memory with the capacity of 32Kwords x 2 channels. Collected data are utilized for data processing and analysis.

(b) Remote machining from irradiated RPV steels In case of irradiated material, since all of manipulation must be handled remotely, machining of the mechanical test specimen should be performed accurately in accordance with the material testing standards such as ISO, ASTM and JIS. However, the remote machining with high accuracy has never been done up to date because the requirement is quite difficult. Therefore, the original machine for general use is modified according to some requirements from radiation environment, free maintenance and higher performance. Moreover, the innovational techniques are applied to achieve the allowable machining by means of remote handling. A numerically controlled machine tool is selected and developed as the most useful apparatus for hot cell work without a human error. As shown in Figure 6, a computerized numerical control (CNC) milling machine developed is composed with the main body for machining and a control system included a personal computer. The machining programs developed in the RHL are a Charpy impact test specimen type A of 10 x 10 x 55(mm) so-called V-Charpy, a plate type tensile test specimen with parallel part of 22.95LX 3Wx 3t(mm), and a three point bending type fracture toughness test specimen with knife-edges.

(c) Remote system technology for fatigue testing One of the important research subjects on the LWR fuel cladding performance at extending burnup is to understand the mechanical properties. The RHL developed an electro-hydraulic fatigue testing machine with two kinds of load cells and servo valves in tandem and in parallel respectively. By exchanging the test fixtures with remote handling, the machine is utilized for a high-cycle fatigue test with arc-shaped specimen machined from LWR fuel cladding, a low-cycle fatigue test with round specimen from structural materials, a crack propagation test and a high-frequency test. Moreover, tensile test, plain strain fracture toughness test and the fatigue pre-cracking for fracture toughness specimen are also possible.

-29- JAERI-Conf 99-009

Figure 6. Computerized numerical control (CNC) milling machine

4. CONCLUDING REMAKS

As described above, the DHL is actively carried out in a wide range of PIEs and are being contributed for the advance of R&D works in JAERI. The development of new and advanced PIE techniques is now very important from the viewpoint of progress of innovative and basic researches as well as R&D in nuclear energy.

5. ACKNOWLEDGEMENT

The authors wish to express their sincere thanks to the staffs of Department of Hot Laboratories for performing PIEs and useful discussions.

- 30 JAERI-Conf 99-009

6. REFERENCES

1) T. Kodaira, T. Yamahara, T. Sukegawa, Y. Nishino, H. Kanazawa, H. Amano and M. Nakata ; HPR-349 "Current Status of PIE Techniques in RFEF", Enlarged HPG meeting (Lillehammer, Norway, 1998)

2) K. Harada, N. Mita, Y. Nishino and H. Amano ; "Development and Application of PIE Apparatuses for High Burnup LWR Fuels", Third JAERI-KAERI Joint Seminar on PIE Technology (Oarai, Japan, March 25-26, 1999)

3) M. Nishi, M. Kizaki and T.Sukegawa; "Development of PIE Techniques for Irradiated LWR Pressure Vessel Steels", Third JAERI-KAERI Joint Seminar on PIE Technology (Oarai, Japan, March 25-26, 1999)

- 31 - JAERI-Conf 99-009

1.4 CURRENT STATUS AND FUTURE PROSPECTS OF JMTR HOT LABORATORY

Osamu BABA, Norikazu OOKA and Taiji HOSHIYA

Department of JMTR, Oarai Research Establishment, JAERI Oarai-machi, Higashi-ibaraki-gun, Ibaraki-ken, 311-1394 Japan

ABSTRACT A wide variety of post-irradiation examinations (PIEs) for research and development of nuclear fuels and materials to be utilized in nuclear field is available in three kinds of (3 — y hot cells; concrete, lead and steel cells in the JMTR Hot Laboratory (JMTR HL) associated with the Japan Materials Testing Reactor (JMTR). In addition to PIEs, re-capsuling including re- instrumentation on the irradiated specimen is currently conducted for the power ramping tests of the LWR fuels using the Boiling Water Capsule (BOCA) or for the re-irradiation tests in the different neutron fields (coupling irradiation test). The newly developed techniques by the JMTR HL have provided us with the key information about the irradiation effects on mechanical and physical properties of the specimen in various environments as fission and fusion reactors. These techniques are focused on several topics as follows; (1) miniaturized specimen test as an advanced mechanical test, (2) slow strain rate tensile test (SSRT) and crack propagation measurement in high temperature and pressure water for the study of Irradiation Assisted Stress Corrosion Cracking (IASCC) of LWR core internals, (3) handling technique on materials containing tritium for the research and development of tritium breeders and neutron multiplier for fusion reactors, (4) jointing method using the conventional Tungsten Inert Gas (TIG) welding for re-assembling of irradiation capsules and/or re-fabrication of specimen, and (5) Nondestructive examination using ultrasonic wave and infrared thermography for the quantitative evaluation of irradiation embrittlement of structural materials in fission and fusion reactors. As there are various PIE facilities around Oarai site, mutual exchange of PIE information, interchange of researchers and mutual utilization on PIE facilities are desired to raise the scientific and technical potential on PIE and to get the break-through of the study in the field of nuclear applications.

INTRODUCTION The JMTR HL associated with the Japan Materials Testing Reactor (JMTR) was put into service in 1971 to examine specimens irradiated mainly in the JMTR. A wide variety of PIEs

- 32 JAERI-Conf 99-009 for research and development of nuclear fuels and materials is available in three kinds of P - 7 hot cells in the JMTR HL. These examinations are on LWR high burn up fuels subjected to power ramping tests, NSRR test fuel, structural materials for LWRs, HTGRs and fusion reactors, shape memory alloys and others. In addition to PIEs, re-capsuling including re-instrumentation [1] is currently conducted for the power ramping tests using the Boiling Water Capsule (BOCA) [2] or for coupling irradiation tests [3]. The newly developed techniques by the JMTR HL have provided us with the key information about the irradiation effects on mechanical and physical properties of the specimen in various environments as fission and fusion reactors. In this paper, the facilities of the JMTR HL are described. Current PIE activities and advanced PIE techniques in the JMTR HL are also presented.

FACILITIES AND FUNCTIONS Figure 1 shows the process of PIE for irradiation sample in the JMTR HL. The JMTR HL is located adjacent to the JMTR, and the irradiated capsules can be transferred through a canal. Some of the irradiated specimens and radioisotope (RI) drawn out from the capsules in the JMTR HL are supplied to the hot laboratory of Tohoku University and RI production facility of JAERI, respectively. In addition, a lot of fuel rod segments, which have been irradiated in power reactors and transported to the JMTR HL, are transferred through a canal to the JMTR after re- instrumented and re-assembled into new capsules in the JMTR HL. Figure 2 shows the arrangement in the ground floor of the JMTR HL. Three trains of 3 - y cells, i.e. 8 concrete cells attached with 4 microscope lead cells, 7 lead cells and 5 steel cells are available for PIEs on irradiated fuels and materials. No a type of cell for MOX fuels is provided. Six globe-boxes for handling tritium-containing materials can be used for the study of fusion blanket. Dismantling irradiated capsules, re-capsuling, re-instrumentation, destructive and nondestructive examinations, microstructure observations of fuel and material specimens are performed in the concrete cells. The lead and steel cells are used for many kinds of material tests such as tensile test, Charpy impact test, miniaturized specimen test, SSRT, stress corrosion cracking test, fatigue test, fracture toughness test, creep test and so on. Furthermore, a scanning electron microscope (SEM) is installed in the lead cell to observe the fracture surface of the tested specimens.

CURRENT PIE ACTIVITIES IN THE JMTR HOT LABORATORY 3.1 Re-instrumentation for fuel of the light water reactor The information on FP gas pressure and centerline temperature of fuel rods during power transient is very important to realize load-following operation and achieve high burn up of LWR fuels. Special techniques on re-instrumentation of FP gas pressure gauge and/or centerline thermocouple were developed in 1990 and 1994, respectively and have already been put into service for the BOCA. Figure 3 shows the re-instrumentation procedures of a center-line thermocouple to an irradiated fuel pellet. This technique consists of several steps; fixation and freezing the irradiated fuel pellets, drilling to make a center-hole, removing of small tips of pellets

-33- JAERI-Conf 99-009 during drilling and welding the top cover attached an FP pressure gauge and a centerline thermocouple.

3.2 Slow strain rate tensile testing (SSRT)forthe study of Irradiation Assisted Stress Corrosion Cracking (IASCC) By the SSRT method, the susceptibility of the irradiated specimen to the stress corrosion cracking (SCC) can be evaluated under the environment of high temperature and high-pressure water. The experiment device for SSRT has a tensile-test machine, an autoclave and a water circulating system with a water purification system as shown in Fig. 4. The IASCC susceptibility and fracture morphologies are obtained from the fractions of SCC area, which are measured by a remote-controlled scanning electron microscope (SEM). In the recent study of IASCC susceptibility, the dependence of the type 304 and 316 stainless steels to IASCC susceptibility on alloy composition, neutron fluence and dissolved oxygen is reported using SSRT experiments [4].

3.3 Miniaturizing testing It is very important to develop material testing technology with miniaturized specimens (0.1 to lmm in minimum dimension), especially for the development of fusion reactor materials. An ion-accelerator base intense high-energy neutron source has been planned to build for the irradiation tests for the development of fusion reactor materials. Because of the limited volume available for the irradiation by an ion-accelerator, the miniaturization of the specimens is inevitable. In addition, this technology is beneficial for reducing radioactive wastes and efficient use of surveillance test specimens of LWRs. Developments of remote operation techniques and equipment are necessary due to the limited manipulation in the hot cells. Developments of the small punch test machine [5], electrical discharge machining device and a computer-aided micromanipulator for handling the miniaturized specimens have been successfully carried out at the JMTR HL. By using the small punch testing apparatus shown in Fig. 5, the load-displacement curves are obtained from the punching force and the displacement of the puncher. The deformation of the specimen is similar to that of the bulge test. From the analysis of the curves, ductile to brittle transition temperature, fracture toughness and so forth are suggested to be obtained. Furthermore, the research and development on hardness test, impact test and so forth with miniaturized specimens have been carried out as the future techniques.

3.4 Tritium handling Beryllium is a candidate for neutron multiplier and plasma-facing material in fusion reactors, and beryllium irradiation studies have been performed to obtain engineering data for blanket design. The most important point of PIE for beryllium is to manage tritium released from irradiated samples. Figure 6 shows a new facility for PIE of irradiated beryllium in the JMTR HL [6]. This facility consists of four glove boxes, a dry air supplier, a tritium monitor and

-34- JAERI-Conf 99-009 removal system, and a storage box for irradiated samples. Maximum amount of tritium to be handled in the facility is 7.4 GBq/day"1.

3.5 Welding technique Welding technique in hot cells is one of the key issues to support the PIE. In the JMTR HL, four kinds of welding techniques have already been developed to fabricate (1) new capsules with irradiated specimens for re-irradiation tests(re-capsuling technique), (2) new specimens from irradiated and tested materials for re-irradiation, (3) instrumented fuel rods from irradiated ones as the FP gas pressure gauge and thermocouple for measurement of centerline temperature (re-instrumentation technique), and (4) Co-60 source from irradiated reactivity adjusting elements in the JMTR.

FUTURE PIE TECHNIQUE 4.1 Achievement ofPIEs in short turn-around time Shortening the turn-around time for PIE is one of the key issues to improve the utility of the JMTR HL. For this issue, the following items are thought necessary. (1) Establishing automatic machines for time consuming tests and pre-test procedures such as high and/or low temperature Charpy impact test sample polishing for metallography etc. (2) Modularize PIE apparatus for quick replacement and installation. (3) Modification of PIE apparatus for easy and quick decontamination.

4.2 Application of advanced NDT technique Continuous monitoring on mechanical and/or physical property changes of the same samples through neutron fluence is not possible with destructive testiness. Many samples from the same material are usually prepared and used for this purpose accepting some error included using different samples. From this point of view, nondestructive testings (NDTs) can be a powerful tool to trace these changes induced by neutron irradiation on the same sample, if the correlation between the parameters affecting NDT characteristics and these properties becomes clear. According to a preliminary research using ultrasonic wave tests (UTs) [9], changes in ultrasonic velocity and attenuation coefficient have found some correlation with embrittlement of materials by fast neutron irradiation. Figure 7 shows the schematic diagram of the ultrasonic wave measurement system installed in the lead cell of the JMTR HL to examine the characteristics of the ultrasonic wave for the irradiated small specimens, used Charpy test ones. It may be possible that NDT can be applied to evaluate some mechanical properties of irradiated specimens, although NDT is normally used as a detecting tool for the defects. In the JMTR HL, the application of NDT technology to PIEs is thought very effective and desirable from the view points of monitoring the same samples, saving testing time, rad-waste management and so on.

- 35 - JAERI-Conf 99-009

FUTURE PERSPECTIVES OF JMTR HOT LABORATORY There are many PIE facilities around Oarai site as shown Fig. 8. Mutual exchange of PIE information among these facilities, interchange of researchers and mutual utilization of PIE facilities are very desirable to raise the scientific and technical potential in the irradiation research and to get break-through of the study in the field of nuclear application.

ACKNOWLEDGEMENT Authors would like to acknowledge to colleagues in the JMTR HL for the support of this presentation.

REFERENCES [1] M. Shimizsu, J. Saito, K. Oshima, Y. Endo, T. Ishii, T. Nakagawa, S. Souzawa, K. Kawamata, Y. Tayama, H. Kawamura, H. Sakai and R. Oyamada, JAERI-Tech 95- 037(1993) 185 (in Japanese). [2] Department of JMTR, Annual Report of JMTR FY1996 (Apr. 1, 1996 -Mar. 31, 1997) , JAERI-Review 98-004, p20. [3] Department of JMTR, ibid., p50. [4] T. Tsukada et al., Proceedings 7th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors, Vol. B (1997) p795. [5] M. Ohmi et al., J. of the Atomic Energy Soc. of Japan, Vol. 39, No. 11 (1997) p966-974 [6] E. Ishitsuka et al., Fusion Engineering and Design 41 (1998) pi95-200 [7] T. Shikamaetal., Nucl. Instr. and Meth. B 91 (1994) 342-345 [8] N. Sekimura, JAERI-Conf 97-006 (1997) 137-143 [9] T. Ishii and N. Ooka, Proceedings of EC-IAEA Specialist Meeting (1999-3)

-36- I Flow of Irradiation Sample

HL of Tohoku Fuels Materials R Univ. Hot Laboratory- (HL)

> m 2 n ri Hot LaboraioP. o

O o Re-irradiation of Fuels and Materials

* Re-instrumentation Machining TC&FP pressure gage Welding J{ ' Capsuling Post Irradiation Examination rradiafion

Fig. 1 Flow diagram of PIE for irradiation sample _rv J—qpj f Service Area Hoi Mock-Up Radiation Dark II Preparation I gaKS Rmim Loading Dock Management 111—I S-2 S-l JRoom J..Berylliu. m r\^l Characteristics Operation stee! Cells Area . Lead Cells Office

Durk IJControl Service Area Room n n rv^ . n

9 JMTR-

Tinnrrf tf Tr TTTT T 6 Microscope Concrete Cells O Lead Ce!ls Operation Area

JMTR Hot Laboratory:

(I 1 2 3 4 5 6 7 8 » Kim I , I . i , I , i , [ , I i I i I , I , I Fig.2 Functional Area of JMTRHL Hz

Removing of Freezing Drilling UO2 chips > en to dual 1 instrumentation- O device O 0 o II U n n o a N2 "IT" o GOO Xe Kr| He! Inserting of Sleeve thermeeouple ing out inserting

Fig. 3 Re-instrumentation procedures of themocouple to irradiated fuel rod JAERI-Conf 99-009

Water makeup system Monitoring/purification system

Ion exchanger

Drain out .—C i DO

pH Cond,

High pressure Pressure SSRT autoclave pump regulator

Cooler •JCUUH'I! /Accumulator MJS316 (ID Safety 1.71 valve

High pressure filter r c~ Heat exchanger

Preheater External reference electrode On top of hot cell L- High temp./press.circulation system Hot cell

Fig.4 Schematic flow diagram of IASCC test facility.

40 Load cell Extensometer

Punching rod Load celf Vacuum

.or

> en n o

© o Push rod for Af specimen clamp en !UiUCi Size of body height: 1.73m width : 0.73m length : 0.66m

Fig.5 Remote controlled SP testing machine JAERI-Conf 99-009

Storage box Exhaust Tritium process monitor blower

GB-5 GB-1 GBJ-2/3 GB-4 Dry air supplier )V3

GB-6 Tritium removal system GB : Glove box V : Changing valve of normal and tritium removal mode — Normal mode ~ Abnormal mode ( after detecting tritium leakage )

Fig.6 Ventilation system at Be PIE Facility

Manipulator

J Data processing unit

Ultrasonic test instrument Clamping rig of probe v

Probe -

Irradiated charpy impact specimen

Fig.7 Schematic view of experimental apparatus for nondestructive evaluation of irradiation embrittlement in hot cell.2

-42- JAERI-Conf 99-009

Accelarator HTTR JMTR

Collaboration of PIE facilities

JNC ' J . i FMF AGF MMF

LWR LWR Fusion High burnup fuel RPV Blanket Material R MOX fuel Core internal Advanced material

Oarai Res. Est.

Tohoku Univ. IJOYO(JNC) NFD

MMF(JNC)

University—National laboratory—Private laboratory

Cooperative research, Research exchange, Mutual facilities utilization, Information exchange etc.

Fig.8 Cooperation of post irradiation examination facilities

43 - JP9950626 JAERI-Conf 99-009

1.5 OVER VIEW OF POST-IRRADIATION EXAMINATION FACILITIES FOR FUELS AND MATERIALS DEVELOPMENT OF FAST REACTOR

Masahiko Itoh O-arai Engineering Center, Japan Nuclear Cycle Development Institute 4002 Narita-cho, Oarai-machi, Higasiibaraki-gun, Ibaraki, 311-1393

Abstract

The hot cell complex for post-irradiation examination of the fast reactor fuels and materials was constructed and has been operated at the o-arai engineering center of Japan Nuclear Cycle Development Institute. The complex Consists of three hot cell facilities. They are the Fuel Monitoring Facility (FMF), the Alpha-Gamma Facility (AGF) and the Materials Monitoring Facility (MMF). The FMF is located adjacent to the experimental fast reactor "JOYO" and started operation in November 1978. In this facility, nondestructive examination of fuel subassemblies and other core components, in addition to some destructive examination of fuel and absorber pins, are carried out. The selected pins and materials, sectioned to the appropriate size at the FMF, are sent to the AGF and the MMF for further detailed examinations. The AGF has been operated successfully since October 1971. The functions of this facility are the physical, metallurgical and chemical examinations of irradiated plutonium-bearing fuels. The MMF was constructed at 1972 and has been operated since 1973 for the reactor materials. In this facility, various tests are conducted on core materials, structural material and control rod materials irradiated in fast reactor. Structural materials irradiated in JMTR and pressure tubes irradiated in prototype advanced thermal reactor "Fugen" are also examined.

INTRODUCTION In the fast reactor, core fuels and materials are exposed in severe environment comparing to thermal reactor. For the commercial application , it is vitally necessary to improve the performance of fuels and materials. The Power Reactor and Nuclear Fuel Development Corporation was established in 1968 .(restructuring to Japan Nuclear Cycle Development Institute (JNC) at October, 1998) Since 1968, irradiation experiments on fuels and materials have been performed in overseas reactors and Japan materials testing reactor (JMTR), while the construction

- 44 - JAERI-Conf 99-009 of post-irradiation examination facilities in O-arai engineering center had also been promoted. The alpha-Gamma Facility (AGF)° for the fuel examination, the Materials Monitoring Facility (MMF)2) for reactor materials examination and the Fuel Monitoring Facility (FMF)36) for the examination of core components of experimental fast reactor "JOYO" were constructed and started operation in 1971,1973 and 1978 respectively. The core modification from the breeding core (MK-1 core) to the irradiation core (MK-n core) was performed in 1982 . Irradiation of fuels and materials in MK-n core was started in 1983. Special devise for irradiation was developed, that is reloaded type irradiation vehicle which is describe elsewhere in detail71. To examine a lot of material specimens in the irradiation vehicle, Material Monitoring Facility was extended and the operation of extended facility was started in 1983. The prototype fast breeder reactor "Monju" reached its fast criticality in 1994. To evaluation of irradiation performance for core component of "Monju", Fuel Monitoring Facility was extended . The construction of extended Facility was started in 1991, and completed in 1995. Pre-operational test for the facility is underway . In JNC , it was established the plan of the Advanced Nuclear Fuel Recycle which aims to reduce the burden of geological disposal by separating long-life nuclide such as Neptunium , Americium and Curium (Minor Actinides) in spent fuels and burning as the Minor Actinides fuels . MA containing fuels have high radio-activity , so it is necessary to fabricate remotely. Therefore, it was planed to install the fuel fabrication apparatus in the hot cell in AGF. Installation of MA containing fuel fabrication apparatus was completed in1998. The functionary tests for the apparatus is underway.

FUNCTION OF POST-IRRADIATION EXAMINATION FACILITIES The role of the post-irradiation examination facilities in O-arai Engineering Center is to examine the fuels and materials irradiated in "JOYO" and other fast reactors for the development of high performance fuels . The fuel performance test and surveillance test of structural materials for "JOYO" are also conducted . Furthermore , surveillance test for the pressure tubes of advanced thermal reactor "Fugen" is conducted in MMF . The outline of post-irradiation examination facilities is as follows.

Fuel Monitoring Facility The facility has four stories above ground and two stories underground.The layout of the first floor is shown in Fig.1. FMF is divided into two area , FMF-1 and FMF-2. The three main concrete cells .Examination cell, Decontamination cell and Clean cell, in FMF-1 are located in first floor. These cell's wall is made of heavy concrete. The shielding capability of the wall facilitates the examination of fuels and materials of 6X 1016Bq for gamma ray in the examination cell. The metallography cell with steel shielding

- 45 - JAERI-Conf 99-009

is also located in the first floor. Specimen transfer is carried out with a pneumatic transfer tube interconnected between the decontamination cell and metallography cell. The handling activity of this cell is 1.1X1013Bq for gamma ray. Another concrete cell for the X-ray radiography of assemblies is provided in the second basement under the examination cell. The Examination cell, Decontamination cell and Metallography cell are large a - y type cells . The Clean cell and radiography cell are 0 - y type . The atmosphere of

Examination cell is maintained as high purity nitrogen with H2O and O2 being less than

100ppm .Metallography cell is also nitrogen atmosphere with H2O and O2 being less than 500 ppm . In FMF-2 , The two main a-y type concrete cells , Examination cell and Decontamination cell, are located in first floor and the /? - y type X-ray CT cell is located in the second basement The a-y type concrete cell's wall is made of heavy concrete . The shielding capability is 6.7X1016Bq for gamma ray. The examination cell is maintained of high purity nitrogen atmosphere. The role of this facility is as follows . • non-destructive examination and disassembling of "JOYO" core component • Metallography of fuel pin • Preperation of the sample for AGF and MMF The post-irradiation examination items for hot cells are shown in table 1.

Alpha-gamma facility The main functions of this facility are fuel burn-up analysis .physical property measurement, chemical analyses for MA elements in MOX fuel and MA bearing MOX fuel fabrication . The layout of the first floor is shown in Fig. 2 . The facility is three stories high with basement. The hot cells are located on first floor. The inner box-type cell is a characteristic, in which air tight stainless steel movable boxes are installed in radiation shielding such as concrete , lead , etc. The specimens are accepted using a transfer container at the No.1 cell. Inter-cell transfer is provided by a conveyer installed under the inner boxes. The specimens transfer from concrete cell to lead cell are carried out with apneumatic transfer tube which is installed between No.7 cell and No. 13 cell. The shielding capability for gamma ray is 1.6X1014Bq for No.1 cell to No.3 cell, 2.6X 1013 Bq for No.4 cell to No.7 cell and 2.6X 1012 Bq for No.11 cell to No.18 cell. The main post-irradiation examination items are shown in table 2.

Materials Monitoring Facility The main functions of this facility are the evaluation of irradiation effect for mechanical properties, physical properties , microstructure for reactor materials. The layout of the first floor is shown in Fig. 3. The facility is two stories high with basement.

- 46- JAERI-Conf 99-009

This facility is divided into two area , MMF-1 and MMF-2 . MMF-1 has six concrete cells (one is located in basement) and two lead cells . The No.1 concrete cell is a - y type, the other are /3 - y type . The front wall for the cells from No.1 cell to No. 3 cell is made of heavy concrete and others are ordinary concrete .The shielding capability of each cells for gamma ray of "'Co is shown in table 3. In the laboratories , the physical properties measurement apparatus are provided . MMF-2 has four concrete cells and one iron cell. one concrete is divided into two parts by stainless steel wall shown in Fig.3. No.1 cell and No.2-1 cell are a-y type and another cells are j3 - y type. It is possible for two a-y type cells to change the atmosphere of air to nitrogen . The shielding capability for gamma ray of ^Co is 1.8X 1013 Bq for No1 to No.4 cell and 3.7 X1013 Bq for No5 cell. To evaluate the microstructure of core materials, transmission electron microscope with accelerate voltage of 400keV is provided in the EM laboratory . The main post-irradiation examination items are shown in table 4.

POST-IRRADIATION EXAMINATION After the criticality of "JOYO", the examination of fuels and materials irradiated in "JOYO" have been performed mainly . The "JOYO" core component such as core fuel assembly, control rod , reflector etc. and irradiation rig are transferred to the FMF. After non-destructive examination , the assemblies are dismantled and sectioned to the small segments to transfer to other facilities . The post-irradiation examination flow is shown in Fig.4 . Up to now, 63 fuel assemblies, 21 irradiation vehicles with fuel pin , 18 control rods , 39 irradiation vehicles for material etc. are provided to post-irradiation examination . The results of post-irradiation examination contribute to fuel design for "JOYO" and "Monju". Furthermore ,15 surveillance test rigs for "JOYO" and 14 surveillance capsules for "Fugen" were also provided to post-irradiation examination , the results was used to confirm the integrity of reactor pressure vessel and pressure tube , respectively.

CONCLUSION Post-irradiation examination facilities in O-arai engineering center, JNC, are described. These facilities have been operating successfully since operations were started. Irradiation performance of the "JOYO" fuel design was confirmed through its PIE results. The fuels and materials development of the fast reactor is being steadily progress in JNC . Further research and development for fuels and materials is being pursued to utilize the PIE facilities.

- 47 - JAERI-Conf 99-009

REFERENCE 1) K.Uematsu , Y.lshida , S.Kobayashi and J.Komatsu ; Proc. 22nd Conf. "Remote Systems Technology", 1974, pp.3-10 2) K.Uematsu , Y.lshida , K.Suzuki; pp11-19 in reference 1 3) K.Uematsu , Y.lshida , S.Seki and T.Hayashi; pp.20-29 in reference 1 4) T.ltaki, T.Shimada and H.Tachi ;Proc. 30th Conf. "Remote Systems Technology vol.2", 1982,pp.16-23 5) S.lwanaga , Y.Nakamura , T.Nagamine and A.Koizumi; Proc. International Conf. "Fuel Management and Handling ", Edinburgh, BNES,20-22,March,1995,PaperNo.56 6) T.ltaki, J.Komatsu S.Yamanouchi and Y.Enokido ; pp24-31 in reference 4 7) K.Maeda , T.Nagamine , Y.Nakamura , T.Mitsugi and S.Matsumoto ; This Seminar, 25-26, March, 1999

Table 1 Function of Cells in FMF

Area Function

Visual Examination Profilometry Gamma Scanning Exam. Cell Pin Puncturing Dismantling and Sectioning Strage Can Welding FMF-1 Decon. Cell Decontamination for In-cell Equipment Clean Cell • Reassembling for Irradiation Vehicle

Metallography • Microstructural Analysis Cell

Radiography Cell • X-ray Radiography

• Visual Examination • Profilometry Exam. Cell • Gamma Scanning • Eddy Current • Dismantling FMF-2 • Strage • Reassembling for Irradiation Vehicle Decon. Cell • Decontamination for In-cell Equipment

X-ray CT Cell • X-ray Radiography and X-ray Computer Tomography

-48- JAERI-Conf 99-009

Table 2 Function of Cells and Laboratries in AGF

Area Function No. 1-1 • Inspection of MA Containing MOX fuel No. 1-2

No 2 • Storage No 3-1 • Fuel Fabrication Concrete No 3-2 Cell No 4 • Sample Preparation for Physical Property Measurement No 5 • Sample Preparation for Metallography No 6 • Sample Preparation for Chemical Analysis No 7 • Transfer by Pneumatic Tube No 8 • Decontamination of In-cell Device No 9

No 11 • Microchemical Analysis No 12 • Metallography No 13 • Transfer by Pneumatic Tube No 14 • Analysis for Fission Product Released from Lead Fuel Cell No 15 • X-ray Analysis

No 16 • Density Measurement No 17 • Melting Temperature Measurement

No 18 • Thermal Diffusivity Measurement

Chemical Laboratry • Chemical Analysis for MA

Physical Laboratry • Analysis of MA (ICP-AES)

Laboratry • Burn-up Measurement by Mass Spectroscopy

Table 3 Handling Activity of cells in MMF-1

Shielding Materials Radioactivity Area of front wall (Bq)

No.1 Heavy Concrete 9.7X1012

No.2 Heavy Concrete 3.7X1013

No.3 Heavy Concrete 4.2X1012

No.4 Ordinary Concrete 1.8X1012

No.5 Ordinary Concrete 3.1X1012 No.6 Lead 1.5X1011

No.7 Lead 1.7X1012

No.8 Ordinary Concrete 3.7X1013

-49- JAERI-Conf 99-009

Table 4 Function of Cells and Laboratories in MMF

Area Function © Cladding Test Cell • Mechanical test for fuel cladding • loading , unloading Loading Cell © Machining Cell • Specimen preperation ® Metallurgy Cell • Specimenn preperation for metallurgy © Mechanical Test Cell • Mechanical test for structural materials

MMF-1 © Microscope Cell • Optical microscope observation © Uniaxial Creep Cell • Uniaxial creep test for structural materials

Storage Cell • Specimenn storage

Gas Analysis • Retaind gas analysis Room

Physical • Thermal conductivity mesurement Laboratory • X-ray diffraction analysis

No. 1 Cell • Fuel removal from cladding

No. 2-1 Cell • Decontamination

No. 2-2 Cell • loading , unloading

No. 3 Cell • Creep-fatigue test for structural materials MMF-2 No. 4 Cell • Dimensional measurement • Density measurement • Visual examination

No. 5 Cell • Uniaxial creep test for structural materials

EM Room • Microstructural analysis by transmission electron microscope

-50- JAERI-Conf 99-009

LAJt-J LJ LAJ Operation Corridor

1 \ / \ / \ / \ / \ 1 \ / \ Examination Cell Jecontamt- Clean - lation Cell Celt Fxamination Cell Decontami- \ / \ / \ / \ / \ / \ / \ / \ 1 \ 1 \ \ natior Cell

Operation Corridor Service Area \i \ i \ i \i \ i \ i \ in Operation Corridor

lAHAf Maintenance Room

T_OT_

FMF-1 FMF-2 Fig . 1 Layout of the Fuel Monitoring Facility

Ventilation and Power Supply

I

lOm

Fig . 2 Layout of the Alplr-Gamma Facility

- 5i - JAERI-Conf 99-009

I LAJ> MMF-1

MMF-2

Fig . 3 Layout of the Materials Monitoring Facility

AdvancedThermal Reactor "Fugen"

I I

I Control Rod | R Pressure Tube

Fuels Monitoring Facility FMF

Assembly Parts, Controll Rod I and Structural Material

i J Materii

Fuels

Materials

Fig . 4 Flow Sheet of Irradiated Fuels and Materials

-52- JP9950627 JAERI-Conf 99-009

1.6 (a) ACTIVITIES OF OARAI BRANCH IMR OF TOHOKU UNIVERSITY AS AN OPEN FACILITY FOR UTILIZING JMTR

Minoru NARUI1, Tsutomu SAGAWA2, and Tatsuo SHIKAMA1

1 Oarai Branch, Institute for Materials Research, Tohoku University, Oarai, Ibaraki, 311-1313 Japan 2 Oarai Research Establishment, Japan Atomic Energy Research Institute, Oarai, Ibaraki, 311-1394 Japan

ABSTRACT

Hot cell facilities in a university open facility of Oarai Branch of IMR, Tohoku University (Oarai Branch) will be described briefly, for general aspects and a beta-gamma handling facility. A related topics concerning alpha-gamma facility will be described in a separate paper. Hot cell works in Oarai Branch is related strongly with utilization of Japan materials Testing Reactor (JMTR) in Oarai Research Establishment of Japan Atomic Energy Research Institute. Steady efforts are made to develop advanced techniques for studies of nuclear materials utilizing a JMTR and its related hot cells in Oarai Branch and JAERI. One of examples will be mentioned in the paper. Acquisition of systematic irradiation data is essential for understanding fundamental processes of irradiation effects and for establishment of reliable database of irradiation effects in fusion reactor materials. It will take several years with expensive several different irradiation rigs in a fission reactor irradiation. There, it will take seriously long time to carry out needed iterations between irradiation tests&evaluation and materials developments. An irradiation rig was developed to carry out irradiation in multiple conditions of temperatures and irradiation fluences. Irradiation tests of fusion reactor materials were successfully carried out in JMTR.

INTRODUCTION

A university open facility of Oarai Branch of Institute for Materials Research in Tohoku University is working for materials study utilizing Japan Materials Testing Reactor in Oarai Research Establishment of Japan Atomic Energy Research Institute. Major playing theaters for promoting researches are

-53- JAERI-Conf 99-009 development of radiation techniques and development of post irradiation examination techniques with miniature specimens. Oarai Branch is furnished with two hot laboratories, one for beta-gamma emitting materials and the other for alpha-gamma emitting materials. They are operated under intimate collaboration with the JMTR and its hot cells. The first part of the present paper will describe general architecture of Oarai Branch for study of nuclear materials and show general schema of beta-gamma facilities. The alpha-gamma facility will be described in a separate paper presented in this seminar[l]. The rest of the paper will mainly focus on the newly developed irradiation technique. An appropriate control of irradiation conditions in a fission reactor[2] is needed to obtain reliable database which can be analyzed in comparison with other irradiation data obtained in different irradiation sources such as charged particles irradiation [3]. However, controlled irradiation is expensive and time-consuming in a fission reactor and it will take more than several years to obtain data in irradiation conditions covering needed range of parameters. Also, realization of the same irradiation in different irradiation rigs in different irradiation cycles is not a easy work in a fission reactor, where existence of other irradiation rigs will change a local neutron flux and a gamma heating rate. A irradiation rig which can realize multi irradiation parameters was developed and controlled irradiation of fusion reactor materials was successfully carried out in Japan Materials Testing Reactor (JMTR) in Oarai Research Establishment of Japan Atomic Energy Research Institute. Ten irradiation conditions were realized in one pseudo-shroud-type irradiation rig in JMTR. The present paper describes a detailed structure of developed rig and a history of successful irradiation. Examples of results of analyses of irradiated fusion reactor materials will be found elsewhere [4].

HOT CELL FACILITY IN OARAI BRANCH

Interests of researchers in universities in Japan have a wide-range spectrum from development of fission nuclear fuel recycling system and development of new materials for advance nuclear systems such as a nuclear fusion reactors to fumdamental studies such as activation analyses. Various kinds of materials are irradiated in JMTR and they must be handled in hot cells in Oarai Branch. Irradiated capsules are disassembled in a hot cell in the JMTR and subcapsules were transported to Oarai Branch. Hot cell facility in Oarai Branch is separated into two parts, one for handing beta-gamma emitting materials and the other for handling alpha-gamma emitting materials. Fig. 1 shows a layout of Oarai Branch. Irradiated beta-gamma emitting materials are handled in the beta- gamma laboratory in Fig. 1. There, subcapsules are opened and specimens are identified and

- 54 - JAERI-Conf 99-009 sorted and they are delivered to each researcher. Fig. 2 shows a layout of the beta-gamma laboratory, which has 6 small lead-shielded hot cells. Researchers prefer to use miniature specimens for restriction of irradiation space and reducing radioactivity. Thus, hot cells are designed to handle these small specimens. Some of material-testings are carried out in the hot cells. Examples are sharpy-tests and tensile tests. Major parts of PIEs are carried out, out of hot cells, as specimens do not have strong radioactivity. Details of hot cells and related works have been already described in the first and second Korean/Japan seminar [1],

Figure 1 Layout of Oarai Branch of IMR of Tohoku University

- 55 - JAERI-Conf 99-009

Waste Measuring Room Room

Service Area Storage Room Isolation Room 1 0 ® 0 Control Loading Dock H Room Steel Cells nn _r Operation Area Lead Cells Changing Room Radiation Management Roon Entrance Office Office

Figure 2 Layout of beta-gamma laboratory with 6 hot cells

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DEVELOPMENT OF IRRADIATION RIG

Figure 3 shows general structures of present irradiation system. Ten small subcapsules were accommodated in a temperature controlled irradiation rig [3], which has independently regulated two temperature zones. The irradiation rig, a protecting tube, a junction box, and a lifting device are forming a psudo-shroud system and the small subcapsules could be lifted up from and inserted down into the temperature controlled rig in the JMTR core, during a reactor operation. Irradiation temperatures were controlled by electric heaters encased in the rig as shown in Fig. 3. Two different temperature zones were set up above and below of the midplane of reactor core, which could be independently controlled irrespective of the reactor power. Figure 4 shows cross sectional view of the rig accommodating the subcapsules. Five transfer tubes were installed in the rig, being thermally bonded by aluminum block. The electric heaters were coiled on the outer surface of the aluminum block, which ensures temperature homogeneity . A reflecting tube and a gap between the reflecting tube and a wall of rig (described as outer tube in Fig. 4) will setup appropriate heat-removal rate for temperature controls. Schematic view of a train of two subcapsules is shown in Fig. 5. Two subcapsules were connected through alumina made thermal insulator and they could be inserted to or removed from the irradiation rig during a reactor operation. Temperature of each subcapsule was monitored by a thermocouple inserted into an aluminum made top cap of the subcapsule shown in Fig. 6. Each of two subcapsules could be irradiated at different temperatures otherwise in nearly the same irradiation conditions.

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Capsule control panel Junction box ^ Lifting device \

Lead out tube

Vacuum tube

F/M Specimen Transfor tube I Insulator TIG / Irradiation rig T/C Electric eater

Thermal bond

Sub capsule

Reflecting tube

(T)~@ : Control : Full cycle

Figure 3 Schematic view of pseudo-shroud irradiation rig developed forcontrolled fission reactor irradiation.

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Reflecting tube Electric heater (SUS304,t=0.7)

Transfer tube Specimen

72 Thermal bond (A1050)

Outer tube Sub capsule (<*> 5.7X04) (<*>40x36.8)

Figure 4 Cross section of irradiation rig accommodating 5 trains of subcapsules

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Wire (SUS304)

Sub capsule (A1050) : Control(removal during cycle) : Full cycle

Arrangement of Transfer tube Insulator (AQ2O3) Figure 6 Cross sectional view of a subcapsule in a transfer tube. Irradiation temperature is monitored by thermocouple at top cap.

)~@ : Control(Removal during cycle) D : Full cycle

Arrangement of Transfer tube

Figure 5 Outlook of a train of two subcapsuels for tow different temperatures

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HISTORY OF IRRADIATION TESTS

The present irradiation rig has a potential of temperature control by changing helium gas pressure in a gap between a reflecting tube and outer tube shown in Fig. 4, independently of the reactor power (gas-pressure-temperature control; GPTC). Figure 7 shows one example of temperature control by this GPTC method, without using electric heaters at the reactor shutdown. The gamma heating rate was changing from about 7W/g to less than lW/g, but the temperature of a subcapsule could be kept constant at about 680K. However, the reactor power changed fast by abrupt insertion of stopping control rod at the end of reactor shutdown and the temperature could not be controlled well by the GPTC. In general, the GPTC has advantages over the electric-heater-temperature-control (EHTC). A structure of rig could be simple and more specimens can be irradiated. The most important to point out is that an electric heater has always a possibility of failure. Although electrical heaters could occasionally survive more than one year irradiation in JMTR ( 5 cycles in a year in average), up to more than 1021n/m2 fast (E>lMeV) neutron fluence, their reliable life-time will be a-few-cycles JMTR irradiation. Development of fusion reactor materials are demanding irradiation exceeding 1022 n/m2 of fast neutron fluence. The GPTC will not have a life limitation as far as a geometry of the gas gap is not changed drastically by the swelling.

500 r

400

33 to 300 O I re

100 -

0 50 100 150

Time from start of shutdown (min)

Figure 7 Example of temperature control by GPTC at reactor shutdown

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38h(9.Q8X1018n/cm)t 92h(2.20X10 n/cm) t 19 186h(4.45X10 n/cm') 354K8.46X10 n/cni) 20 590h(1.41X10 n/cm)

673K 573K (Improved Temperature Control)

Control lMay,8(19:50) 50MW ! Control Start (Reactor Power) JUN,2(10:30) Stop

QMW OMW T May,8,96(9:57) JUN,2(12:30)

Figure 8 Irradiation history using the present rig. Subcapsules were inserted into and removed from the rig during reactor operation.

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(X/zCi)

Fluence Monitor

u 250 500 750 1000 (mm) T3 C [From Core Center]

Figure 9 Results of dosimetry of fast neutron fluence as a function of distance from midplane of reactor core. - 63- JAERI-Conf 99-009

However, the GPTC can not control abrupt change of a reactor power in the present system because it takes several minutes to attain equilibrium gas pressure in the gas gap. The basal temperature control was carried out by the GPTC and the EHTC was used for compensating abrupt but small change of temperature especially at the reactor start and shutdown. Figure 8 shows temperature history of irradiation using the present irradiation rig in 1996. The subcapsules were inserted into the irradiation rig after the reactor power and the temperatures of the rig were stabilized as shown in Fig. 8. Then, subcapsules were sequentially removed from the rig during the reactor operation. Irradiation with five different levels of neutron fluence from 9xlO22n/m2 to 1.4xlO24n/m2 at two different temperatures of 573 and 673 K were realized in one exertion of irradiation. A previous preliminary results, however, suggested that specimens were exposed to low flux fast neutron irradiation even when they were not inserted in the reactor core. Figure 9 shows induced radioactivity of iron dosimetry foil as a function of a distance along the height of reactor core. The induced radioactivity is roughly proportional to the fluence of fast neutron. It can be seen that substantial neutron flux exists even in an out-of- core-region. A length of the rig was enlarged as long as possible and the subcapsules were placed at about 300mm above the edge of the reactor core to avoid exposure to the low flux neutrons, where the fast neutron flux is about 10-4 of that at the core center. More than a few thousands TEM (Transmission Electron Microscope) specimens of different fusion candidate alloys were irradiated. Microstructural modifications due to a fission reactor irradiation were examined in comparison with those under other irradiation sources such as high energy electrons in HVEMs (High Voltage Electron Microscope) [4], where extensive data were accumulated and fundamental processes of irradiation induced microstructural evolution was analyzed as a function of a variety of irradiation conditions.

CONCLUSION

A rig was developed for controlled irradiation in JMTR fission reactor. Irradiation of five different fast neutron fluence at two different temperatures could be carried out successfully using the developed rig. History of irradiation confirmed the well-control of temperature and neutron fluence.

References

l.M.Narui, et al., The 2nd KAERI-JAERI Joint seminar on PIE technology, Sept. 20-22, 1995, Taejon, Korea. P.242 2. Y.Suzuki et al., presented in this seminar.

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3. M.Kiritani et al., J. Nucl. Mater, 191-194 (1992) 100 4. M.Narui et al., J. Nucl. Mater., 212-215(1994)1645 5. N.Yoshida, presented in the ICFRM-8 (Int. Conf. on Fusion Reactor Materials) Sendai, 1997.

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1.6 (b) VENTILATION SYSTEM OF ACTINIDES HANDLING FACILITY IN OARAI-BRANCH OF TOHOKU UNIVERSITY

Yoshimitsu SUZUKI, Makoto fATANABE, Mituo HARA.Tatsuo SHIKAMA, (Hideo KAYANO) .Toshiaki MITSUGASHIRA

Oarai-branch, Institute for Materials Research, Tohoku University Narita-machi,Oarai-machi, Higashi ibaraki-gun, Ibaraki, Japan

ABSTRACT

We have reported the development of the facility for handling actinides in Tohoku University at the second KAERI-JAERI joint seminar on PIE technology. Actinide isotopes have most hazurdous a-radioactivity. Therefore,a specially designed facility is necessary to carry out experimental study for actinide physics and chemistry. In this paper, we will describe the ventilation system and monitoring system for actinide handling facility. INTRODUCTION

The Oarai-branch of Institute for Materials Research in Tohoku University has been an open facility to researchers in Japanese universities who want to utilize irradiation service in the Japan Materials Testing Reactor (JMTR) of the Oarai Laboratory of the Japan Atomic Energy Research Institute since its foundation in 1969. To meet increasing interest in studies on actinide physics and chemistry,a new laboratory for actinides experiment(LAE) was constructed during 1987-1991. In order to promote experimental works on actinides research, it is neccessary to insure the health physical protection system for the daily use of alpha-emitters. LABORATORY FOR ACTINIDES EXPERIMENT

The LAE is three stories high with one basement and has earthquake-proof structure made of reinforced concrete. Most of the experimental equipment is settled in the first floor. Figure 1 shows a layout of the first floor, i. e., main hole of LAE. Radiation protection area(RPA), shown in bold line, is divided into two zones,a low level zone and a high level zone. The rooms for contamination test, radiometry, physical characterization, and cell operation are in the low level zone and samples enclosed in proper vessels or capsules are treated in these rooms.

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Thus, these rooms are regarded as contamination free area. In the rooms of pyrochemistry and solution chemistry, unsealed actinide samples are treated and these rooms are called as umber rooms. Handling of highly radioactive materials is performed in the hot cell and precise experiments are carried out in the rooms of solution chemistry and pyrochemistry by using glove boxes or drafthoods.

Mass Flow of Actinide Research A small quantity of TRU has been produced from commercially available actinides such as U,Np,and Am by neutron irradiation in JMTR. Materiales for the irradiation are also prepared in LAE. The materials are encased in a sealed subcapsule usually made of fused silica which is then encapsulated into a stainless steel clad for a short term irradiation in hydraoulic rabbit or a stainless steel capsule-rig for a long term irrsdiation. Every enclosure is examined by X-ray autoradiography before irradiation and transported to JMTR. After the irradiation, the rabbit or the rig is cooled in a water pool in JMTR to wait for the decay of short-lived induced radioactivities. Then, the subcapsule is retrieved in a hot cell in JMTR and transported to LAE by using a container applied with thick lead shield. The container is transported into LAE through the loading dock and settled onto the transfer port, named gamma-gate, of storage cell by using a 10 tons crane. The gamma-gate has an air tight structure applied with 250 mm thick lead shield and the irradiated subcapsule can be transferred into the storage cell. The irradiated actinide containning specimen is retrieved by using a cutter in the storage cell and then transferred to the working cell through a transfer port which consists of a pair of double-sealed and air-leak-tight doors on each side of the two cells. The chemical separation of TRU is carried out in the working cell and the isolated TRU is transferred to the cell glove box attached on the side wall of the working cell. Then, TRU thus isolated may contain impurities of other actinides and lanthanides. The final purification to remove these impuritiesis carried out in the room for solution chemistry by using a glove box or a draft-hood. Sometimes, commercially obtained actinides contain impurities. The removal of these impurities is also performed by using these equipments.

Specification of Hot Cell Figure 2 illustrates the structure of the hot cell. The cell shield is made of 350 mm thick SS-41 steel and the inside of the shield is covered with polished lining made of 4mm thick SUS 316L plates. Each SUS 316L plate was welded together to make air-leak-tight structure of the two cells. Seven air-tight manipulators (Sargent Model-L), five lead glass windows,250 mm thick lead equivalent, and a control desk are attached in the front wall of the two cells. Major experiment in the working cell can be carried out by using four manipulators inspecting the

- 67 - JAERI-Conf 99-009 inside condition through one of the three windows. The setting of the experimental apparatus inside the cell can be made by using a glove port attached at the rear side of SUS lining wall. Many feed-throughs are available to get easy access for electricities, gases and chemical reagents. An isolation room is provided for the maintenance and decontamination of apparatus settled in the cells. The room also has air-tight structure and the maintenance works will be done appling a tunnel suit attached to the tunnel port. These maintenance works will be supported by supporters in service room. Air in the isolation room is taken from hot area through a gallery attached at the wall of service room and transported through one of the two overhanged HEPA filter cases. Another HEPA filter case is equipped at the rear wall of the cell shield to transport the air into the cells. Air ducts are attached to each filter case to insure the down blow of the air.

Radiometry [J Physical L Characterization

Figure 1. Layout of the LAE

-68- JAERI-Conf 99-009

MAINTENANCE GLOVEBOX FOR MANIPUtATORS

[SERVICE ROOMl

URTtGHTDOOR TUNNEL PORT

WASTE PORT I

IISOLAT1ON ROOMl

WALL UNING (SS41 350mm) DOOR (SUS-316L 4mm)

TUNNEL PORT \GLOVE POR

Figure 2. The structure of the hot cell

For the cleaning of the exhaust from the cell, cell filters are also equipped and the exhaust is treated finally by using a filter assembly of hot cell. The filter assembly is consisted from two ULPA filters and one chacorl filter. The ULPA filter can remove 99. 999% of airborne radioactive particles of 0.0001 mm in diameter. Leak-tight automatic-valves are attached to the cell ventilation system. These assemblies can sustain a pressure difference upto 500 mmAq. The measured leak rates are less than 0. 01 volX/h and less than 0. 007 volVh for the cells and cell glove box, respectively.

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Maximum Limits of Main Actinide Nuclides for Daily Use

Table 1 shows maximum permissible amount of main actinide nuclides which can be used in LAE. To keep maximum freedom and to minimize the official inspection due to NPT, the amount of Pu is restricted to be less than lg/y. The actinide elements which can be used in substantial study of solid state physics and chemistry are Th, U, Np, and Am. The conceptual design of health physical protection system and monitoring system is made to sustain the experimental use of these nuclides.

Table 1. Maximum limits of main actinide for lailc y use Nuclide In hot cell In glove box 226Ra 400 GBq 10 MBq 2 3 2^ (500 g) (1,000 g) irrad. Th 750 GBq (100 g) 10 MBq ( 50 g) 231Pa 20 GBq ( U.4 g) 50 MBq 233U (100 mg) ( 40 mg) 2S5JJ 5 GBq 500 MBq 238U (500 g) (1 000 g) irrad. U 750 GBq (100 g) 10 MBq ( 50 g) EU«20X) ( 15 g) ( 5 g) HUO90X) ( 50 mg) ( 20 mg) 237Np 5 GBq (191.52 g) 200 MBq 2 3 8pu 20 GBq 20 GBq 2 3 9pu (200 mg) ( 100 rag) 24 'Am 200 GBq ( 1. 57 g) 5 GBq 243Am 40 GBq ( 5. 41 g) 5 GBq 24ZCm 500 GBq ( 4. 07mg) 100 MBq 243Cm 200 GBq (104.61 rag) 500 KBq 244Cm 100 GBq ( 33. 35mg) 100 KBq 248Cm 50 MBq (327. 78mg) 100 KBq 251Cf 2 GBq ( 34.12mg) 40 MBq 252Cf 50 MBq ( 2. 5 Hg) 100 KBq 253Es 20 GBq ( 0. 8 fg) 200 MBq

Ventilation System of LAE

LAE has maximum 100,000 m3/h once through ventilation system, and usually operate at about 50,000 m3/h. Inlet air is taken through role type dust filters and salt removing filters by using three ventilators settled in the cold-ventilator room at the third floor of LAE. The inlet air is introduced into RPA through three air lines,low level line,hot area line,and umber line. The air in the low level area

- 70 - JAERI-Conf 99-009 is passed into the hot area and a small portion of the air in the hot area is introduced into cell lines as explained in former section. The exhaust from the hot area and umber rooms is transported to one of the 9 filter cases, each of which is consisted with a prefilter and two stage of ULPA filter that has the ability removing 99.999% of 0.1// particle. The air in umber room is partially introduced into draft hoods which are attached with two stage alkaline scrubers. The exhaust from these scrubers is also transferred into the same filter cases. All the filter cases and fans for exhaust are settled in the basement floor. The outline of these ventilation system is shown in Figure 3. Pneumatically controlled valves and dumpers are attached on each ventilation line and the pressure in the RPE is always controlled below atmospheric level. The conditions of air flow as well as the status of valve operation can be seen in a display board settled in the control and monitoring room. All exhaust is released from 40 m tall stack after the monitoring of alpha and beta-gamma radioactivites contained.

o;u GLOVE BOXES

I :::-•»••::. I f K u :y

-e- LAB -e- AIR EA INLET R:ROLL FILTER WASTE S:SALT CLEAR FILTER P:ME FILTER C:CHARCOAL FILTER STORAGE -J H:HEPA FILTER U:ULPA FILTER HOT -e- AREA P!H

I .•:•••••*»-••••. l P :.' CELL 1 t v ••

CELL 2 P:'c -©-

WASTE -e- AIR WATER INLET

EXHAUST P-H Figure 3. The outline of ventilation system

- 71 - JAERI-Conf 99-009

MONITORING SYSTEM OF LAE

The monitoring system of LAE is composed of in-cell monitors,exposure rate monitors for RPA, air line monitors,and exhaust air monitors. The specifications of these monitors are shown in Figure 4. All monitors are connected to a large display board settled in the control and monitoring room. Variable alarm level setting is possible for each monitor from the display board. Once the alarm is raised, inter-lock protection, such as the shut-down of the fans and alarm rings for workers, are automatically triggered.

In-Cell Monitor and Exposure Rate Monitor

Each cell is equipped with an ionization chamber to inspect the exposure rate. If it exceeds the alarm level, inter-lock system is triggered to prohibit opening shielding doors and the maintenance works in the isolation room. It is neccessary to cancel the alarm condition by using manipulators. Usually, the maximum of the exposure rate in the RPA is controlled to be lower than 0. 001 mSv/h. The exposure rate monitors are settled in high level zone and continuous monitoring is made regardless of experimental works.

Air Line Monitor

A SSB detector, a Nal scintillation detector and a GM counter are applied to the air line sampling system in LAE to monitor continuously the dust trapped on the surface of a filter. The signals from the SSB are recorded in an analyser which calculates the real alpha contents subtracting radon daughter contributions. In spite of this substraction ability, back-ground level of the alpha counts from SSB changes according to the condition of ventilation system. Thus,the filter is exchanged daily and the alpha-counts are measured separately by using a- spectrometer in order to confirm the contamination free atmosphere in LAE.

Monitors for Exhaust

The exhaust which passes through ULPA filter is bypassed to the monitoring system. The monitoring system for exhaust is equipped with five detectors and a dust sampler as shown in Table 2. This monitoring system is very important to ensure the non-release of radioactive substances into environment. Two ZnS detectors are applied to measure the contents of alpha radioactivity in the dust continuously collected on the role-type filter sampler. One is used to measure the dust just after the sampling and the other is used to measure about 24 hours later to wait for the decay of the signals due to 222Rn daughters. Actualy, the sensitivity about

-72- JAERI-Conf 99-009

MONITORING SYSTEM OF LAE

a, 0, 0 • 7 ST A C K D U ST •G A S MO N IT OR CONTROL

a, 0 ' 7 PANEL RO OM DU ST •G A S MON IT 0 R

7 j DATA ; AR E A MO N IT 0 R i TREATMENT:

7 1 DISPLAY 1 I N C E LL M 0 N IT 0 R : & • •' PRINT-0UT1 a, 0, 7 WA ST E WA T ER MO N I T 0 R

Figure 4 Monitoring system of LAE

STACK DUST-GAS SAMPLER

SAMPLER DETECTOR RADIOACTIV RAY MEASURING PROCEDURE Zn S a 1 JUST AFTER SAMPLING

DUST Zn S a 2 1 DAY AFTER SAMPLING

PLAST I C 0'7 JUST AFTER SAMPLING I ON I ZAT I ON 0 REAL TIME, CONTINUOUSLY GAS C HAMBER

Na I 0'7 IODINE REAL TIME, CONTINUOUSLY

Table 2 Stack dust-gas sampler

- 73 - JAERI-Conf 99-009

10 Bq/cm3 is attained by using this system. Main component of these alpha- counts is due to the daughters of220 Rn which may be generated in the concrete of LAE and fluctuates according to the humidity.

Monitoring of Waste Water

In LAE, the washing for cleaning experimental tools is prohibited. Thus, the water mainly comes from scrubers. All waste water is stored in one of the four tanks, each has a capacity of 4 m3. The monitors of waste water are equipped but have never been operated, because the total volume of the waste water generated during these 7 years is less than 3 m3. Instead, sample is taken periodically into a 1, 000 cm3 marineri-beaker and gamma-ray spectrum is inspected. After the inspection of the gamma-ray spectrum,alpha-contents are measured by using SmF3 coprecipitation technique or liquid scintillation spectrometry combined with pulse shape discriminator. We have developed a new type extracting scintillator for the selective extraction of TRU. The main component of the extracting scintillator is 20 vol% TBP-toluene, which contains 0. 02g/cm3 of naphthalene and 4 mg/cm3 of PBBO. The water sample is mixed with calcium nitrate tetrahydrate to be the IhO/Ca ratio less than 8 and the salt solution is shaken with an equal volume of the extracting scintillator. All TRUs can be extracted quantitatively and the organic phase can be applied to the accumulation of alpha-spectrum.

Reference

Suzuki, Y. ;Hara, M. ;Shikama,T. ;Mitsugashira, T. ;Kayano, H. 1990:Application for Permission of Uses of Radioactive Materials and Nuclear Fuel Materials to the Science and Technology Agency of Japanese gaverment. Suzuki, Y. ;0chiai,A. ;Shikama, T. ;Mitsugashira, T. ;Kayano, H. 1995: Development of Facility for Handling Actinides in Tohoku University. KAERI-NEMAC/TR-32, 90-100

- 74 - JP9950629 JAERI-Conf 99-009

1.7 PIE ACTIVITIES IN NFD HOT LABORATORY

Norikatsu Yokota, Keizo Ogata and Noriyuki Sakaguchi

Nippon Nuclear Fuel Development Co., Ltd. 2163 Oarai-machi Narita-cho, Higashi-Ibaraki-ken Ibaraki-ken, 311-1313, Japan

ABSTRACT

Nippon Nuclear Fuel Development Co., Ltd. (NFD) has been operating hot laboratory facility since 1977 for post-irradiation examinations (PIE) of boiling water reactor (BWR) fuels and structural materials. Various examination techniques have been developed to meet the research requirements. The BWR fuel design, which has been revised for a step-by-step burnup extension, has been verified at each step through comprehensive PIEs. A large number of fuels and materials have been examined in various research and development programs. High burnup fuel pellets were extensively examined in terms of fission gas behavior and microstructural evolution. Cladding waterside corrosion performances were studied from a viewpoint of the base metal metallurgical conditions. An electro-chemical technique was applied for determining oxide film characteristics. Reactor core structural materials have also been studied for plant life extension and development of remedies.

INTRODUCTION

Nippon Nuclear Fuel Development Co., Ltd. (NFD), a subsidiary of Hitachi and Toshiba, has been operating hot laboratory facility since 1977 for extensive post-irradiation examinations (PIE) of boiling water reactor (BWR) fuels and structural materials. NFD hot laboratory has a capability to accomodate full size commercial BWR fuel bundles. Comprehensive PIE programs have been carried out on many BWR fuel bundles [1-4] including failed fuel bundles [5] and MOX fuel bundles[6], as well as test fuel and material specimens irradiated in test reactors. To meet the demands for detailed mechanistic understanding of fuel

-75- JAERI-Conf 99-009 performance, more precise microscopic and specific PIE techniques are required. Various examination techniques have been developed during the course of the PIE programs to meet the research requirements. This paper presents the overview of recent PIE activities in NFD hot laboratory.

OUTLINE OF THE NFD HOT LABORATORY

Layout of the NFD hot laboratory is shown in Fig. 1. It consists of a storage pool, an inspection pool, six concrete cells, six steel shielded cells, two waste storage cells, and an isolation area. It has a capability to accomodate full size commercial BWR fuel bundles. Standard PIE procedures include non-destructive examinations followed by destructive ones. A window is installed in the side wall of the inspection pool so that the fuel bundle can be observed directly. Non-destructive examinations on fuel bundle and fuel rods can be performed in the inspection pool and the monitoring cell. Concrete cells, shielded by concrete walls lined with stainless steel sheets for easy decontamination, are used for destructive examinations such as mtallography and ceramography. Steel shilede cells annexed to the concrete cells are used for the tests on relatively small specimens, such as mechanical testings. Various kinds of microscopic equipment, including transmission electron microscope (TEM), scanning electron microscope (SEM), electron probe micro- analyzer (EPMA), mass spectrometer, and X-ray diffractometer (XRD), are installed in precise measurement labs. Special apparatus for specific examinations on irradiated materials, such as thermal diffusivity measurement by laser flash method, post-irradiation annealing, etc., are also installed there.

OVERVIEW OF PIE ACTIVITIES

1. Research and development trends for BWR fuel Burnup extension with the design changes followed in Japanese BWRs is shown in Fig. 2[7]. Following the research activities in the early use of fuel with the focus mainly placed on enhancing the reliability and capacity factor, one of the largest technical efforts during last decade has been burnup extension aiming at reduction of spent fuel amount and improvement of the fuel cycle economy. The BWR fuel design, which has been revised for a step-by-step burnup

-76- JAERI-Conf 99-009 extension, has been verified at each step through comprehensive PIEs[l-4] in terms of the required performance and design margins. A large number of fuels and materials irradiated in commercial reactors as well as those in test reactors have been examined in various research and development programs. Significant amounts of data have been accumulated especially on high burnup phenomena. Utilization of plutonium uranium mixed oxide (MOX) fuel in light water reactors is another important issue in Japan. Programs for the MOX fuel have also been carried out including PIEs on MOX fuel bundles irradiated in a commercial BWR and test fuel irradiations in test re actors [6,8,9].

2. PIEs on fuel pellet andFP'behavior Fission product (FP) gas release and FP gas bubble swelling are of practical importance in determining high burnup fuel performance. Since such phenomena are closely related to the fuel microstructure, irradiation-induced microstructural evolution is also of major interest at high burnup. FP gas release rate of irradiated fuel rods can be measured by both destructive (puncture test) and non-destructive methods. The latter utilizes the measurement of 85Kr gamma activity at the rod plenum. Some FP gas release data[4] are shown in Fig. 3. Fuel rod axial distribution of FPs is measured by gamma scanning in a hot cell. Radial distributions in a fuel pellet cross section are examined with micro-gamma scanning device, EPMA, and ion micro-analyzer (IMA). A large amount of data has been accumulated in the fuel performance database to support development of a fuel performance analysis code which employs mechanistic models of FP gas behavior. FP gas behavior in a fuel pellet was studied using post-irradiation annealing technique [10]. A small specimen of irradiated fuel pellet was heated in the high temperature furnace and the released 85Kr was measured by gamma activity. Typical results are shown in Fig. 4 demonstrating burst FP gas release at some temperature. Further, high temperature and high pressure furnace has been developed[ll] to study FP gas behavior under various restraint pressures simulating restraint force by pellet-cladding interaction (PCI) which could suppress FP gas bubble growth and its release. Fig. 5 shows some results of de- pressurization experiments under isothermal annealing at 1500°C to simulate a rapid removal of PCI restraint. A large burst release was observed immediately after the de-pressurization. Such results are consistent with the irradiation data obtained in power bump tests. Microstructural evolution in high burnup UO2 and U02-Gd20.3 fuel pellets, such as formation of rim structure and pellet-cladding bonding, were extensively examined by detailed PIE techniques utilizing EPMA, XRD, SEM, and TEM[12].

- 77 - JAERI-Conf 99-009

Typical ceramograph, and SEM and TEM images of fuel pellet irradiated to 60GWd/t are shown in Fig. 6[13]. Sub-divided grain structure (rim structure) was seen at the pellet periphery. Its formation mechanism was studied from the detailed examinations as shown in Fig. 7 [14]. Tangled dislocations were organized into sub-grains of 20-30nm in size with high angle boundaries which were regarded as the nuclei for recrystallization resulting in sweeping out of FP gas atoms into small intragranular bubbles. Regions of the pellet-cladding bonding layer of the high burnup fuel above 40GWd/t were examined in detail[15]. AZrO2 layer consisting of cubic polycrystals was found near the cladding inner surface. In a region near the UO2 pellet surface, both a cubic solid solution of (U,Zr)O2 and an amorphous phase existed. The derived formation mechanism of bonding layer is summarized in Fig. 8. A key process is the phase transformation of ZrO2 film from monoclinic phase which is stable at temperatures below 1170°C to cubic phase. This observed phase change is attributed to fission damage.

3. PIEs on fuel cladding materials Cladding waterside corrosion and associated hydrogen pickup are also important issues at high burnup. Oxide thicknesses of the cladding outer surface are measured non-destructively by eddy current method and destructively by metallography. Typical data of oxide thickness are shown in Fig. 9[16]. Fuel rods of recent step II design showed a remarkable improvement in corrosion resistance. Hydrogen contents are measured by hot vacuum extraction method. Corrosion performances of irradiated Zircaloy-2 and other zirconium alloys were studied from a viewpoint of the base metal metallurgical conditions utilizing SEM and TEM[16-18]. Fig. 10 shows schematic illustrations indicating the irradiation-induced change of precipitates in Zircaloy-2 cladding tubes. Zr(Fe,Cr)2 type precipitate in irradiated Zircaloy-2 undergoes crystalline-to-amorphous transition and has Fe-depletion in the amorphous region, i.e. dissolution of Fe atoms from the precipitate to the matrix. Zr2(Fe,Ni) type precipitate also changes its shape and both Fe and Ni diffuse away into matrix. Such radiation-induced dissolution was modeled taking the precipitate size into consideration and calculated as shown in Fig. 11. Dissolution rates of various Zircaloy-2 cladding tubes were estimated and relationship with their corrosion behaviors is also shown in Fig. 11. The dissolution rate has a clear effect on the corrosion performance. An electro-chemical technique was applied for determining oxide film characteristics. The electric resistances of oxide films formed on various Zr alloys in out-of-pile steam and in BWRs were measured utilizing an AC impedance device shown in Fig. 12[19]. Some results are shown in Fig. 13. Impedance

- 78 - JAERI-Conf 99-009 responses differed remarkably between pre- and post-transition oxide films, although TEM observations gave no clear difference in crystal shapes and sizes. The impedance measurement results on various Zr alloys irradiated in a BWR demonstrated that the alloys whose oxide had a lower electronic conductivity showed a better corrosion performance. Mechanical properties of cladding tube are not supposed to significantly change at high burnup, but they should be watched in relation to oxide buildup and hydrogen pickup. Tensile, internal pressurization burst, fatigue and charpy tests are performed in hot cells.

4, PIEs on BWR core structural ma terials Reactor core structural materials have also been studied for plant life extention and development of remedies. Slow strain rate tensile and uniaxial constant load tests have been performed on irradiated specimens under simulated BWR conditions. Microstructures of irradiated stainless steels were examined utilizing TEM equipped with field emission electron gun (FE-TEM) which enabled to analyze microscopic area with the resolution of 1 nm to investigate irradiation- induced defects and segregation affecting the mechanical and chemical behaviors such as irradiation assisted stress corrosion cracking (IASCC).

SUMMARY

The major interest of BWR fuel R&D has shifted to burnup extension. To meet the demands for detailed mechanistic understanding of fuel performance, especially at high burnup, more precise microscopic and specific PIE techniques are required. Various examination techniques have been developed in NFD during the course of the PIE programs to meet the research requirements. A large number of fuels and materials irradiated in commercial reactors as well as those in test reactors have been examined in various research and development programs. Detailed PIEs on fuel pellets, cladding materials, and core structural materials have been successfully carried out and significant amounts of data have been accumulated.

-79- JAERI-Conf 99-009

REFERENCES

1. Y. Mishima and T. Aoki, Proving Test on the Reliability of BWR 8X8 Fuel Assemblies, Paper Presented at IAEA International Symposium on Improvements in Water Reactor Fuel Technology and Utilization, IAEA-SM- 288/58, Stockholm, Sept. 15-19 (1986). 2. M. Oishi, High Burnup Fuel Behavior Studies in NUPEC, Paper Presented at IAEA Technical Committee Meeting on Fuel Performance at High Burnup for Water Reactors, Nykoping (1990). 3. H. Ohara, et al., Fuel Behavior During Power Ramp Tests, Proc. International Topical Meeting on Light Water Reactor Fuel Performance, West Palm Beach, April 17-21 (1994). 4. H. Hayashi, et al., Irradiation Characteristics of BWR Step n Lead Use Assemblies, Proc. 1997 International Topical Meeting on Light Water Reactor Fuel Performance, Portland, May 2-6 (1997). 5. K. Ogata, et al., Post Irradiation Examination on the Failed Fuel Rod in the Hamaoka Atomic Power Station Unit 1, Proc. International Topical Meeting on Light Water Reactor Fuel Performance, West Palm Beach, April 17-21 (1994). 6. M. Ichikawa, et al., J. At. Energy Soc. Japan, 39, 2 (1997) pp.93-111 (in Japanese). 7. K. Ogata, et al., BWR Fuel Performance and Recent R&D Activities in Japan, Proc. 1997 International Topical Meeting on Light Water Reactor Fuel Performance, Portland, May 2-6 (1997). 8. M. Oguma, et al., Technology Development for Japanese BWR-MOX Fuel Utilization, Paper Presented at IAEA Technical Committee Meeting on Recycling of Plutonium and Uranium in Water Reactor Fuel, Newby Bridge, July 3-7 (1995). 9. K. Asahi, et.al., Irradiation and Post Irradiation Testing Program of BWR MOX Fuel Rods, Proc. International Topical Meeting on Light Water Reactor Fuel Performance, West Palm Beach, April 17-21 (1994). 10. K. Une, et al., J. Nucl. Sci. Technol., 27, 11 (1990) p. 1002. 11. S. Kashibe and K. Une, Effect of External Restraint on Density Change and Fission Gas Release in UO2 Fuels, Paper Presented at Enlarged Halden Programme Group Meeting, Lillehammer, March (1998). 12. K. Une, et al., Effect of Irradiation-Induced Microstructural Evolution on High Burnup Fuel Behavior, Proc. 1997 International Topical Meeting on Light Water Reactor Fuel Performance, Portland, May 2-6 (1997). 13. M. Hirai, et al., Performance of Improved UO2 Pellets at High Burnup, ibid. 14. K. Nogita and K. Une, J. Nucl. Mater., 226 (1995) p.302.

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15. K. Nogita and K. Une, Formation Process of Pellet-Clad Bonding Layer in High Burnup BWR Fuel, Paper Presented at IAEA Technical Committee Meeting on Advances in Pellet Technology for Improved Performance at High Burnup, Tokyo, Oct. 28-Nov. 1 (1996). 16. Y. Etoh and S. Shimada, J. Nucl. Sci. Technol., 29, 4 (1992) p.358. 17. Y. Etoh, et al., J. Nucl. Mater., 200 (1993) p.59. 18. Y. Etoh, et al., The Effect of Microstructure on Corrosion Behaviors of Zry-2 in BWRs, Twelfth International Symposium on Zirconium in the Nuclear Industry, Toronto, June 15-18 (1998). 19. S. Nanikawa, et al., Correlation Between Characteristics of Oxide Films Formed on Zr Alloys in BWRs and Corrosion Performance, Twelfth International Symposium on Zirconium in the Nuclear Industry, Toronto, June 15-18 (1998).

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Cross sectional view Inspection window

Concrete cells Pool

Precise measurement labs.

Waste storaae area

• I I chemicat labJS

Steel shielded cells Grand floor olan

Fig. 1 Layout of the NFD hot laboratory

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60 ; 3OOO0O0OO aoooooooo O Water rod ooooooooo ooooooooo * : Small number of step III LUAs ooooooooo ooooooooo T3 OOOO^NOOO OOOf \OOO were loaded in 1996 Qocy-wooo oool looo ©ookjooc - ioL_Jooo CD oooooooo ooooooooo ooooooooo 50 ooooooooo ooooooooo D. oooooooo oooooooo POOOOOOOQi POOOOOOOQ 9X9 (Type A) 9x9 (Type B) C i_ DOOOOOOO ooeUooo 1 D oooooooo STEP-IE (45)* " oooooooo oooooooo OOOOQOOO 40 OOOOOOOO OOOOOOOQ STEP- n (39.5) oooOoooo cd oooooooo o oooooooo STEP-1 (8 x 8BJX33) OOOOOOOQ 8x8RJ(29.5) I © 30 7x7R(27.5)

cd 8x8(27.5) 7x7(21.5) < 1970 1980 1990 2000 Year of loading

Fig. 2 Change of average bundle burnups at discharge

50 • 1 1 •

A,V: conventional 8X8 D :HPF • 40 • O :Step! LUA

a) Black symbol;(U,Gd)O2 w -S> 30 a: to (0 A A| A O 20 • 1I A A ANT g w A OT A A ^ A A 10 M A • D

10 20 30 40 50 60 Rod Burnup (GWd/t)

Fig. 3 Burnup dependence of fission gas release

-83- qq h Restraint pressure (Mpa) era at 00 00 NJ 6o o o O O en 00 w CD P3 CD GO P Temperature (°C) CD Kr-85 activity (Arbitary unit) GO O CD 3 GO Hi 5" era h GO 0 k CD O O > CD en t3 2 B CD n to Hi o H 0 P 3 3_ 3 0 3 CD CD al i CD O O f 00 3 0 era "—'0 "73 0 t3 -p»- O p 0 CO T3 0 & HJ CD p en 13 0 P CD 0 ->• -»• ro GO ST. ^^ o> o GO o o o o C o o o HJ Fractional release (%) 3 P N 3 Temperature (°C) CD O P 3 tn 3 oq JAERI-Conf 99-009

, ( 'ii d subble

, ;tal!izing rngion 'T?V^s-f

Radiation damage 'of- 3a accumulating region | 200nm

Ceramograph SEM images TEM image of the rim region

Fig. 6 SEM and TEM images of fuel pellet irradiated to 60GWd/t

Point defects Cladding inner surface oxidation Interstitials Vacancies (Monoclinic ZrOa)

Fission damage —•( RecombinationJ in ZrO2

Phase transformation of Dislocations Bubbles ZrO2 Monoclinic-*Cubic

Sub-divided grains ^~*\ closure J

L Strong contact of cubic ZrO2 and UO2. Recrystallization

Formation of (U,Zr)O2 solid soliution

Recrystallized grains Coarsened bubbles

Rim structure ing layer

Fig. 7 Formation mechanism of the Fig. 8 Formation mechanism of the rim structure bonding layer

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20 30 40 50 60 Local burn up (GWd/t) Fig. 9 Maximum oxide thicknesses on three types of Zircaloy-2 cladding tubes irradiated in BWEs

TEM images TEM images

Fe I Low o 15 i fluence 'a. 'o ' "o I Q. ^ Crystal 03

| Medium Fe Ni Fe I fluence T3 C 03

/Amorphous c o High fluence b

Zr-Fe-Cr type precipitates Zr-Fe-Ni type precipitates

Fig. 10 Schematic illustrations indicating the irradiation-induced change of precipitates in Zircaloy-2 cladding tubes

86- JAERI-Conf 99-009

1°.4 Particle size : 0.25 urn Measured (a) Dissolution rate ' Calculated as a function of U 0.2 neutron fluence •£

4 6 8 10 12 14 Fast neutron fluence (E>1MeV, x 1025 n/m2)

(b) Relationship between oxide thickness and dissolution rate

10-9 10-8 Initial dissolution rate of Fe+Ni (at%/s)

Fig. 11 Dissolution rate of Fe from precipitates in Zircaloy-2 and relationship between oxide thickness and dissolution rate of Fe+Ni

Working electrode (Specimen) Lock-in amplifier

Reference T electrode Potentiostat (Ag/AgCI)

\ T Personal computer Counter electrode (Pt)

Control unit

Fig. 12 Block diagram of the AC impedance measurement system

-87- • Zircaloy-2 • Pre-transition A High FeNi/Zry-2 • Post-transition O 0.5Nb/Zry-2 10 10 10 10 • i a a B CD 8 CD 10 OL 10 — a. D) CD 13 o O 10° CD 106 CD to Li k x— 10* 104

2 >rn 10' 10 N 2 0 n 0) 0) o 3 CD CD • -30 Z3 -30 6 > o cb~ % CD" 1 ^0O O 2 • ^^ 3 % CD -60 CQ -60 1 CD CD CD Jll I, 1 -90 -90 10" 10u 10' 10" 10"4 10* 10u 10' 10" Frequency (Hz) Frequency (Hz)

(a) Unirradiated Zry-2 (b) Irradiated for 4 cycles (Oxide film formed out-of-teactor) (Oxide film formed in-reactor)

Fig. 13 Typical results of impedance measurements JAERI-Conf 99-009 JP9950630

1.8 Current Status of NDC Fuel Hot Laboratory

Youichirou YAMAGUCHI1, Takanori MATSUOKA1, Satoshi SHIRAISHI1 Mitsuteru SUGANO2

1 .Hot Laboratory Experiment Department, Nuclear Development Corporation Tokai-mura, Naka-gun, Ibaraki-ken, Japan 2:Nuclear Fuel Engineering Department, Mitsubishi Heavy Industries, Ltd. Wadasaki-cho, Hyogo-ku, Kobe, Japan

ABSTRACT

Nuclear Development Corporation(NDC) fuel hot laboratory was established to investigate the causes for leaked rods and to confirm the integrity of the precedence irradiation fuels, in 1986. After that, it obtained a license to conduct PIE of the structural materials, such as stainless steels, inside the reactor in addition to fuels. So far we have conducted PEE of fuels and metallic materials including fuel assembly components and reactor internal components irradiated in Japanese PWR plants or some test reactors. To meet these PIE needs, we are making efforts to improve facilities and to install high advanced equipments. This paper describes current status of the facilities and PIE techniques in NDC fuel hot laboratory.

INTRODUCTION

As hot laboratories to conduct PIE, NDC is equipped with the fuel hot laboratory and the material hot laboratory. Each has /? - y cells, and we can handle nuclear fuel substances in only fuel hot laboratory. The fuel hot laboratory has been established to investigate the causes for leaked rods, to confirm the integrity of the precedence irradiation fuel, and so on. In recent years, fuel leakage does not occur in the domestic PWR plants. The current major works are the PIE related to research and development of high burnup fuels and reactor internal component materials against the background of PWR plant life extension. Implementation of PIE for about lOyears caused increase in the volume of waste generated in the fuel hot laboratory, and this resulted in

-89- JAERI-Conf 99-009 additional installation of a waste storage warehouse in 1996. In the material hot laboratory, PIE for the surveillance test in the PWR nuclear reactor vessel steel has been conducted since 1972. This laboratory has mainly been used in mechanical tests such as Charpy impact test and tensile test. The material hot laboratory is also used to conduct a performance test of charcoal filter used in the nuclear power plant. In addition to these hot laboratories, NDC has the fuel test facility to manufacture of unirradiated pellets on a trial basis and to perform initial characteristics tests, and the facility to test the unirradiated fuel assembly structure. This paper describes the equipments and PIE techniques paying attention to the fuel hot laboratory of these facilities.

1. Current Status of the fuel hot laboratory As shown in the layout of Fig 1, the fuel hot laboratory has a pool, six cells and two instrumental analysis rooms. Table 1 shows the cell specification, and Fig. 2 shows the PIE flow classified according to test sites. (l)Pool Almost all the PIE samples are supplied from the PWR plants or test reactors. A fuel assembly or fuel rods are transported in the cask called MSF-1 which contains one fuel assembly, as illustrated in Fig 3. The fuel assembly or fuel rods are replaced from the transport cask to the specified position within the pool by the pit crane. In the case of fuel assembly, the fuel rods to be tested is removed from the assembly after the top nozzle is removed by electrical discharge machining in the pool. Then the fuel rods are loaded into No.l cell for PIE. In addition, the pool is also used to store assemblies and fuel rods as well as high level waste. It is also possible that the high level waste, which is shielded by dry cask, is stored in the warehouse on the ground except the pool. The pool is also be used for appearance test and oxide film thickness measurement. Layout of the pool is shown in Fig.4. (2)No.l cell No. 1 cell is used for non-destructive test of fuel rods. About 10mm length from the upper end of the fuel rod is clamped, and inspection is carried out in the vertical direction. So three fuel rod drive units that go up or down the distance of 4m are located in this cell. The accuracy in the operating distance, when the fuel rod is raised 4m, is within 0.5 mm. An example of the appearance of this drive unit is shown in Fig5. Appearance tests have been carried out by photographing, but this is being switched over to photographing by digital camera in recent years. This makes a significant contribution to speed up. Eddy current test and dimensions measurement have been made by entering

-90- JAERI-Conf 99-009 data into the computer to facilitate subsequent data processing. (3)No.2 cell No.2 cell is utilized for preparation of the sample such as cutting of fuel rods, removing of pellets and reassembling of rods, and sealing of waste into the can. Complicated machining including not only cutting but also grinding and electric discharge machining has been performed. For example, such work includes preparation of tensile samples provided with parallel section because high burnup fuels involve difficult work of removing pellets and preparation of the 3mm-diameter disk sample to measure thermal diffusivity rate for the pellet. The schematic diagram of these machining method and procedure are shown in Fig. 6. (4)No.3 cell No.3 cell is mainly used to conduct the tensile test of the fuel cladding tube and internal pressure burst test or the like. Stress corrosion cracking(SCC) test for non-fuel is also performed in this cell. To perform SCC test in the space within the limited cell, autoclaves under the worktable are installed. The sample pulling mechanisms mounted on the top of the autoclaves are removed at normal times, and is installed for test, thereby ensuring effective use of the space in the cell. Atmosphere of SCC test is the PWR primary simulate water in high pressure and high temperature and it is circulated through the water quality regulator installed out of the cell and inside cell. The appearance of the SCC devices is shown in Fig. 7. (5)No.4 cell No.4 cell is used for the sample preparation of ceramography and metallography and for chemical examination such as the pellet dissolution characteristic tests. (6)No.5 cell No.5 cell is utilized to observe the samples polished and etched in No.4 cell. There are the optical microscopes and the hardness tester in this cell. Negative film was used to take a photograph. Similarly to the case of appearance test in No.l cell, digital camera has been frequently used to photographing in recent years. The data sampled by this are stored in the computer in preparation for immediate transmission to any other places via the network line. (7)First instrumental analysis room There are the hydrogen analyzer, the thermal ionization mass spectrometer(TI-MS) and the field emission transmission electron microscopy (FE-TEM) in this room. TI-MS and FE-TEM have not shields as very small or diluted samples are handled there. TI-MS required to measure the pellet burnup was just renewed in 1998 because of dilapidation of the equipment. Except for sample setting almost all operations are made

- 91 - JAERI-Conf 99-009

automatically, and this makes a significant contribution to manpower saving The hydrogen analyzer has been renewed to improve measuring accuracy and to add He analytical function in 1998. A mass analysis detector has been added to this instrument to sure that He content of metallic materials can be measured. This instrument heated up the sample to 2500°C. Therefore, contamination may be spread out the periphery of the main unit. To prevent this, the main unit is accommodated in the glove box. The appearance of this instrument is shown in Fig8. FE-TEM has been installed to allow observation in very fine area and analysis by energy dispersive X-ray spectroscopy. We have made effort to make a good sample to observe the oxide film on the fuel cladding tube and the rim region in fuel pellets. (8)Second instrumental analysis room The second instrumental analysis room is equipped with a cell having with hexahedral sides called satellite cell. This cell is connected with No.l by a pneumatic tube to ensure easy transport of the sample. 4 devices have been adhered to the sidewall of this cell. These are electron micro analyzer (EPMA), secondary ion mass spectrometry (SIMS), X-ray diffractometer (XRD) and laser flash thermal diffusivity measuring device (L/F) that Nuclear Power Engineering Corporation (NUPEC) was introduced for high burnup fuel verification test. These devices are normally accommodated inside the biological shield. Except for the L/F, they are installed on two rails, and can be pulled out whenever required. The inductively coupled plasma-mass spectrometer (ICP-MS) has been installed to perform chemical analysis related to reprocessing It will be used mainly to measure the isotope of pellets and pellet dissolution residual substance. A mockup test is currently being planned to compare interchangeability between this data and that of TI-MS.

2. Sample management system The samples to be handed in the hot laboratory are required to be placed under severe management not only for the nuclear fuel but also RI samples. In this context, we are preparing a new sample management system that consists of new software and hardware. By this system, the speedy and fine sample management will be anticipated.

3. Summary This paper described the current status of NDC fuel hot laboratory. From now on, we has made further efforts to enhance sample preparation techniques, to offer PIE data featuring a higher measurement accuracy.

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Tablei Specification of hot cell Wall thickness(m) Dimension of cell Radioactivity Hot cell No. Shielding material Front Rear Ceiling (WxDxH)m (max Bq) Heavy concrete 1 No.1 8X3X7.5 3.0 X1015 Ordinary concrete 1.3 1.2 Heavy concrete 1 No.2 5X3X4.5 1.5X1018 Ordinary concrete 1.3 1.1

No.3 Ordinary concrete 1.1 1 1 3X3X4.5 2.0 X1013

No.4 Ordinary concrete 1.1 1 1 3X3X4.5 2.0 X1013

Lead 0.2 No.5 Ordinary concrete 1 3.5X1.5X2.5 3.0 X1012 Iron 0.3

Satellite cell Iron 0.2 0.2 0.2 About 2.5X2.5X2.5 2.0 X1010

-93- Service area Decomtaminiion area

Sample preparation room No.2 Instrumental analysis room

Na n Instrumental o analysis room oI o Sample transfer tube o

raiioii room

LAJ

Fig.1 Layout of the Fuel Hot Laboratory JAERI-Conf 99-009

Location Flow Diagram of PIE

1Storage of Spent Fuel Pool Inspection of Rods Re-assembling (Canal)

Non-Destructive Test Specific Surface Visual Inspection Length & Profile Measurement Area Measurement* No.1 X-ray radiography Cell Oxide Thickness Measurement * Puncture & Gas Gamma Scanninq Eddy-Current Test Ramnlinn

' 1 No.2 Cutting & defueling Welding Electric discharge Cell Grinding machining

Cladding Mechanical Test No.3 Tensile Test Creep Test Burst Test SCCTest* Cell r -• \ Density Measurement SCC Test

-> \ Chemical Separation

No.4 Dissolution Test Cell

W Polishing & Etching

• No.5 Metallography Cell Optical Microscopy Micro Hardness Test

No.1 Hydrogen & Helium r r mSlrUmcnlal Analysis TI-MS Gas Analvsis Analvsis Room TEM

r •1 EPMA* ICP-MS No.2 r Instrumental —^i QrtfAlljfi-* f^iall ^ ^\ OIIVIO / M^O Analysis Room * XRD* \^ • L/F Thermal Diffusivity* * : NU P EC's Devices

Fig. 2 A flow of PIE in the fuel hot laboratory

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Neutron

No.I Cell

Loading unit

-Waste storag< Fuel storage rack rack

6m

4m View from A-A section

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Rod Clamp

Rod Support Roller

i

Fig.5 Appearance of fuel rod drive unit

- 97 - Cooling water

bonded CKttinS a:

(1) Processing procedyre of tensile test specimen

> en 2 to o 00 Sample holder o A section of fuel pellet 3mm 3 O O

Wax

Slice cutting mmammmmM Crack conditions X confirmation by optical microscope observation Processing by diamond cylinder drill

(2) Processing procedyre of fuel pellet for the laser iash thermal diffusivify rate measurement

Fig.6 An example of specimen preparation JAERI-Conf 99-009

Sample pulling mechanism

Autoclave

device 'So.2. device No.

Fig.7 Appearance of the SCC Devices

-99- JAERI-Conf 99-009

Hydrogen analysis Helium analysis con- Shielding Main unit control system trol system \ I

Fig.8 Appearance of hydrogen analyser

- 100- JAERI-Conf 99-009

SESSION 2

PIE TECHNIQUES

ELEMENTARY TECHNIQUES FOR THE STUDY OF POWER REACTOR CHAIR : Y.-S. Kim (Hanyang Univ.)

MICRO STRUCTURAL AND QUANTITATIVE ANALYSIS CHAIRS : T. Matsuoka (NDC) and S.-B. Ahn (KAERI)

ASSEMBLING AND UTILIZATION TECHNIQUES CHAIRS : K. Ogata (NFD) and Y.-S. Choo (KAERI)

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2.1 Development and Application of PIE Apparatuses for High-burnup LWR Fuels

Katsuya HARADA, Naoaki MIT A, Yasuharu NISHINO and Hidetoshi AMANO

Hot Engineering Division Department of Hot Laboratories

ABSTRACT

The Reactor Fuel Examination Facility (RFEF) is developing the following post irradiation examination apparatuses: •Ion Microprobe mass analyzer (IMA) •Pellet Thermal Capacity measuring apparatus (PTC) •Micro Density Measuring apparatus (MDM) •Shield-type Field Emission Scanning Electron Microscope (FE-SEM) The present paper mainly describes several technical topics of these apparatuses.

1 . INTRODUCTION

Extended fuel burnup of LWR fuel is in progress, and the post irradiation examinations (PIEs) of reactor fuels have become very important to clarify the irradiation behavior of high- burnup fuel pellets and cladding tubes. In these contexts, the Reactor Fuel Examination Facility (RFEF) was developing several new apparatuses to obtain the PIE data for confirming the integrity and safety of the high-burnup fuels. Ion Microprobe mass Analyzer (IMA) is used for analysis three-dimensional and isotopes analysis on fuel pellet or micro surface of cladding tube based on the secondary ion mass analysis. Pellet Thermal Capacity measuring apparatus (PTC) is used to measure the thermal capacity of minute fuel pellet specimen based on the thermal flux type Differential Scanning Calorimetry (DSC). Micro Density Measuring apparatus (MDM) is used to measure the micro fuel pellet

- 103 - JAERI-Conf 99-009 density by the immersion density method. Shield-type Field Emission Scanning Electron Microscope (FE-SEM) is used to observe and analyze the micro region. Shield-type FE-SEM uses the Field Emission type electron gun and Energy Dispersive X-ray Spectrometer (EDS) for element analysis.

2 . THE OUTLINE OF EACH APPARATUS

2. IMA Qualitative and quantitative analysis in the micro region have become very important to grasp in detail the irradiation behavior of high-burnup fuel pellets and cladding tubes. Data obtained was strongly needed to clarify the irradiation behavior of high-burnup fuels such as Fission Product (FP) gas release, Pellet-Cladding Interaction (PCI), hydrogen pickup in cladding tube, etc. IMA was developed to analyze depth profile of isotopes on fuel pellet or micro surface of cladding tube in order to clarify irradiation behavior in high-burnup fuel by Secondary Ion Mass Spectrometry (SIMS). SIMS uses a focused primary ion beam to erode atoms from a selected sample region. A fraction of the sputtered sample is emitted as positive or negative secondary ion. A secondary ion emitted from the sample is detected by secondary ion optics, then mass spectrometry is carried out. IMA consists of ion guns, sample system, vacuum pumps, secondary ion optics, secondary electron detector and so on. IMA is covered with shielding for radioactive materials, and measuring operation is remotely performd an outside control section. Schematic drawing of The IMA is shown in Figure 1.

ENTRY CHAMBER x N

SECONDARY ELECTRON^DETECTOFr

[ELECTRON

y TRON ©SAMPLE SECONDARY ION OPTICS FiQ.1 SCHEMATIC DRAWING OF THE IMA

- 104 JAERI-Conf 99-009

The ion gun system has oxygen and cesium ion guns as primary ion source. The oxygen ion gun is used as effectively releasing positive secondary ions for analyzing metal FP, TRU, etc. The minimum diameter of oxygen ion beam is less than 0.6um. The cesium ion gun is applied to release negative secondary ions effectively for analyzing oxygen in the oxide films on the cladding surface and hydrogen in the cladding. The minimum diameter of cesium ion beam is less than 2|im. Objective lens was made to be the plug-in type. It was considered that the contamination by radioactive material discharged from the sample. The secondary ion optics used quadrupolar mass spectrometer, which was simple and compact size. Shielding material made of the tungsten alloy was equipped around the quadrupole in order to decrease the effect on the background by discharged gamma-ray from the sample. The secondary ion lead-in electrode was made to be the plug-in type in order to ease the maintenance. IMA is possible to detect the trace element of ppb level in solid sample, because the secondary ion optics has been equipped with the channeltron. The mass spectrometric analysis is range from 1 to 450 amu. The sample system mainly consists of analysis chamber, entry chamber and sample stage. The sample stage is used by means of the eucentric type. The sample stage can be moved straightly, rotated and tilted, and analyzed within the region of 30mm. The analysis chamber can be evacuated beyond 4x10" Pa in order to analyze Low Mass element such as hydrogen in the cladding tube. Presently, IMA is carried out mock-up examination of sample preparation with small degas, because the measurement is performed on high evacuate condition.

2. 2 PTC The thermal conductivity data is strongly needed for more detailed evaluation of high- burnup fuel behavior. The thermal conductivity is calculated from thermal diffusivity, thermal capacity and density. Until now, the data of the thermal capacity has been using literature data. PTC was developed to measure the thermal capacity of the same small specimen used by the thermal diffusivity measurement and to improve the accuracy of thermal conductivity of irradiated fuel pellet. PTC measures the thermal capacity by heat-flux type Differential Scanning Calorimetry (DSC). The heat-flux type DSC is generally accepted to collect specific heat capacity data in the high temperature region. The basic composition of heat-flux type DSC and the measuring principle of specific heat capacity are shown in Figure 2. The specific heat capacity will be measured as follows: At first, the blank pan and sample pan are put on the holder of heating furnace. Secondly, the temperature is controlled with constant heating velocity. The specific heat capacity can be calculated by the following equation:

n WstxHsa _ + Cp = x Cpst WsaxHst

- 105 - JAERI-Conf 99-009

Where: Wst, the standard sample weight Wsa, the measured sample weight Hsa, the base line shift quantity of the measured sample (Hsa=C-A) Hst, the base line shift quantity of the standard sample (Hst=B-A)

Cpst, the standard sample specific heat capacity at the Tl temperature

SAMPLE PAN(Pt)

HEATING FURNACE

BLANK PAN(Pt)

HOLDER(Pt)

SENSIBLE HOT PLATE BASELINE(STANDARD) 1 BAS ELI N E (SAM P LE) I

THERMOCOUPLE OF TEMPERATURE (TYPE R) OETECTOR OF TEMPERATURE DIFFERENCE RECORDER 1

Fig.2 THE BASIC COMPOSITION OF HEAT- FLUX TYPE DSC AND THE MEASURING PRINCIPLE OF SPECIFIC HEAT CAPACITY.

The PTC consists of sensor unit, base unit, sample preparation unit and shielding box. The PTC is able to be operates remotely for using the irradiated sample. Schematic drawing of the PTC is shown in Figure 3.

HOT CELL 0>HEATING FURNACE J: HOLDER SAMPLE PREPARATION UNIT (PLATINUM) E CHAMBER £ AMPLE ©THERMOCOUPLE (TYPE? R) I J

SENSOR UNITl

PAN(P1A[ IMUM1

COVFR(PI ATINUM)

! SAMPLE

Fig.3 SCHEMATIC DRAWING OF THE PTC The sensor unit is composed of heating furnace, sample pan, sample chamber and sample transfer system. The measuring temperature range is from room temperature to

- 106 - JAERI-Conf 99-009

1500°C. The temperature is measured with typeR thermocouple. The sample pan and sample holder are made of platinum. The sample transfer system can automatically set up a sample to sample holder of which is very weak. The base unit is composed of the electronic circuit for the temperature control and data measuring. The base unit is installed outside shielding box to avoid radiation damage of the electronic circuit. The sample preparation unit is used to pack irradiated fuel pellet fragment for good heating contact. The packed sample can prevent dispersion of radioactive materials. The sample preparation is carried out in hot cell. The measurement data is transferred to the computer, which displays data in real-time and saves. In the data processing, it is possible to carry out specific heat capacity calculation, etc. To verify the performace of the PTC, an experiment has been carried out using platinum sample. Standard sample was A12O3 powder, and measuring sample was platinum wire. The specific heat capacity data was measured in the 100°C step from 200°C to 1400°C at one time. As an example, the measurement result of specific heat capacity of platinum is shown in Figure 4.

0.30

0.25

j: 0.20

E 0.10

0.05 Measuring data Literature data 0.00 200 400 600 800 1000 1600 TEMPERATURE (°O) Fig.4 SPECIFIC HEAT CAPACITYOF PLATINUM

The measuring data was compared with literature data, the each data comparatively good linearity. It was possible to obtain the sufficient data in order to confirm the initial performance in case of platinum, but in case of the shape of the sample changes, the data seems to change. The measurement uses different shape and sample will be carried out in the future for establish preparation method and measuring technique, in order to obtain the high precise data using the high-burnup irradiated sample.

2. 3MDM

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The thermal conductivity data is very important in order to carry out the detailed evaluation of the high-burnup fuel behavior. Until now, the measurement of density was used in the one of fuel pellet fragment of approximately lOg. On the other hand, the sample used in the thermal diffusivity measurement is small pellet fragment less than lOOmg. So that, MDM was developed to measure the density of the same sample and to improve the accuracy of thermal conductivity o f irradiated fuel pellet. MDM is measured by immersion density method, which is little effect for shape and open pore of the sample. The immersion density is measured by buoyancy difference of the sample between in liquid and air. The apparatus construction is simply for maintenance. MDM is composed of weighing unit, liquid tank, sample changing system and shielding box. The MDM can be operated by remote handling in order to use the irradiated sample. Schematic drawing of the MDM is shown in Figure 5.

v j

\ \ 1 1QU1D TANK | vlETAXYLENE r ( ^ATER 1 VIETHYLENE ] ' (,' I (ODfDE

\-—(SAMPLE CATENALY

v_ SAMPLE CHANGING SYSTEM

V. y SAMPLE BASKET

Fig.5 SCHEMATIC DRAWING OF THE MDM Sample catenary is installed in the weighing unit on the hook of the bottom suspension style. The balance readability is 1 n g, and its repeatability is ±0.9 /i g. The liquid tank unit is carried out the gravimetry in the atmosphere and liquid by a vertical motor driven movement. One of water, meta-xylene and diiodomethone is used for the immersion liquid. The sample changing system is automatically hanged for a sample on the bottom suspension hook under the weighing cell. The measuring data of weight and temperature are transferred to the computer and then is processed. The gravimetry data is collected with the presetable condition. It takes only the 10 stable data after the immersion of the sample. The mean value of 8 data except for maximum and minimum are adopted in the measuring data. The temperature data in air and liquid are collected and used for parameter of determining sample density. To verify the performance of the MDM and the weight of sample basket affects the

108 - JAERI-Conf 99-009 measuring result, an experiment has been carried out using nickel sample. The immersion liquid used meta-xylene which osmosis better than pure water. The weight of each sample basket is 318.333mg, 326.374mg and 376.567mg. The sample weight is 61.09mg. As an example, The measurement result of density of nickels shown in Figure 6.

• A:31 8.333m g

• 8:326.374m g

9.1 A C :376.567m g

• D .Literature data

o s t 8-5 T

A B CD Fig.6 DENSITY OF NICKEL

The measuring data was compared with literature (4) data. The measuring data is not affected by the sample basket. It was possible to obtain the sufficient data in order to confirm the initial performance of MDM in case of nickel sample. However, it is necessary to consider that the porous influences in the result, in case of the sample such as a fuel pellet. The density measurement used another immersion liquid and sample will carry out in the future for establish measuring technique, in order to obtain the good result using high-burnup irradiated sample.

2. 4 Shield-type FE-SEM Observation and analysis in the micro region are indispensable to grasp the high-burnup irradiation behavior of cladding tube and fuel pellet. Therefore, shield-type FE-SEM was developed. FE-SEM can observe sample with high magnification, since it has resolution of the submicron order in secondary electron image by using field-emission electron gun. The shield-type FE-SEM consists of electron gun, detector, sample stage, vacuum system, and is possible to operate by remote handling outside shielding box. The electron gun uses the cathode field emission type. Since the illumination of cathode emission type is very higher than the conventional thermionic emission type, so it is possible to obtain high resolution in an equal acceleration voltage. The sample stage is eucentric goniometer type, which able to tilt the sample without changing the focus of the observation position. The vacuum system consists of rotary pump, turbomolecular pump and ion pump.

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FE-SEM is equiped with EDS to identify element. Schematic drawing of the EDS is shown in Figure 7.

o o

LNj TANK

EXHAUST SYSTEM SOLENOID VALVE

DETECTOR

Magnet collimator

PREAMPLIFIER COLLIMATOR

COLUMATOR DRIVEN MECHANISM

MOUNTING FLANGE

• SHIELDING BLOCK

Fig.7 SCHEMATIC DRAWING OF THE EDS

Since sample is irradiated material, therefore, effect of radiation to detector must be reduced to the utmost. The shielding block and collimator made of tungsten alloy were installed at the detector tip in order to reduce the radiation effects and to detect characteristic X-ray with small noise. The elemental analysis can be carried out from oxygen to plutonium. Presently, shield-type FE-SEM is under design and construction. FE-SEM construction will be completed in FY 1999, and performed mock-up measurement.

3. SUMMARY

The RFEF is developing IMA, PTC, MDM and Shield-type FE-SEM to clarify the irradiation behavior of high-burnup fuel pellets. It was performed the characteristic test and possible to obtsin the sufficient data in order to confirm the initial performance of apparatus. It is planned to use these apparatus for PIE of high-burnup fuel in the future.

110- JAERI-Conf 99-009

4. ACKNOWLEDGEMENT

The authors acknowledge to Dr. T Kodaira, director of Department of Hot Laboratories, for his valuable advice. The authors with to express their sincere thanks to the staff of Department of Hot Laboratories for performing experiment and useful discussions, and to the staff of SEIKO EG&G CO., LTD, RIGAKU Corporation, TAIYO Corporation and JEOL LTD for developing new apparatuses.

5. REFERENCES

1) Development of examination technique; JAERI-Review 98-023, PP.51-63 2) Iwanami Shoten Publishers; The physical and chemistry dictionary. P.934. 3) Maruzen co., ltd; The chemistry handbook basic edition 2. PP.214-216 4) Saito, Y; The base of the thermal analysis for material science; P. 107 5) Kodaira. T, Kikuchi. A; Present Status of PIE Techniques in Tokai Hot Cell Facilities; The 5Th Asian symposium on research reactors; May 29-31, 1996, Taejon, Korea

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2.2 A TECHNIQUE OF MELTING TEMPERATURE MEASUREMENT AND ITS APPLICATION FOR IRRADIATED HIGH-BURNUP MOX FUELS

Takashi NAMEKAWA and Takashi HIROSAWA Alpha-Gamma Section, Fuels and Materials Division O-arai Engineering Center Japan Nuclear Cycle Development Institute O-arai-machi, Higashiibaraki-gun, Ibaraki-ken, Japan

ABSTRACT

A melting temperature measurement technique for irradiated oxide fuels is described. In this technique, the melting temperature was determined from a thermal arrest on a heating curve of the specimen which was enclosed in a tungsten capsule to maintain constant chemical composition of the specimen during measurement. The measurement apparatus was installed in an alpha-tight steel box within a gamma-shielding cell and operated by remote handling. The temperature of the specimen was measured with a two-color pyrometer sighted on a black-body well at the bottom of the tungsten capsule. The diameter of the black-body well was optimized so that the uncertainties of measurement were reduced. To calibrate the measured temperature, two reference melting temperature materials, tantalum and molybdenum, were encapsulated and run before and after every oxide fuel test. The melting temperature data on fast reactor mixed oxide fuels irradiated up to 124 GWd/t were obtained. In addition, simulated high-burnup mixed oxide fuel up to 250 GWd/t by adding non-radioactive soluble fission products was examined. These data shows that the melting temperature decrease with increasing burnup and saturated at high burnup region.

INTRODUCTION

The Alpha-Gamma Facility (the AGF) is consisted of equipments for PIE, i.e., twenty one gamma-shielding cells and sixteen glove boxes, and has been operated successfully since 1971. Physical and chemical examination were conducted for the fuel pins irradiated in "JOYO" and overseas reactors such as the Phenix and the FFTF. In a design of fuel pin, temperature of fuel pellet centerline is limited not to exceed the melting temperature of a fuel pellet. During irradiation, the melting temperature of fuel is considered to decrease slightly with increasing burnup due to buildup of soluble fission products in fuel matrix. For irradiated and unirradiated UO2 and (U, Pu)O2 fuels, many workers have determined melting temperatures by so-called V-shaped filament method [1]. However, there have been

- 112- JAERI-Conf 99-009 large variation in the results which might be the change of the oxygen to metal ratio and/or the vaporization of the specimen at high temperature. To avoid these effects, Lyon et al. applied the thermal arrest technique to determine solidus and liquidus temperatures for unirradiated UO2-PUO2 phase diagram [2]. In this technique, an oxide fuel specimen is heated within an sealed tungsten capsule, so that effects of the composition change and vaporization of specimen can be avoided during a measurement. Aitken and Evans also evaluated the melting temperature of unirradiated (U, Pu)O2-x as a function of plutonium content and oxygen stoichiometry, 2-x, using this technique [3]. At the AGF, some apparatus for this technique had been introduced in cells and melting temperature has been measured with good accuracy on UO2 and (U, Pu)O2 fuels irradiated in fast breeder reactor (FBRs), an advanced thermal reactor (ATR), and boiling water reactor (BWRs) for more than fifteen years. This paper describes the melting temperature technique and recent results.

SPECIMEN PREPARATION

Specimens to be examined are both irradiated and unirradiated UO2 and (U, Pu)O2 fuel pellets. At first, fuel pellets are granulated by either drilling or crushing in order to pack the fuel specimen into a tungsten capsule. For irradiated fuel pellets, an irradiated fuel pin is cut into small pieces about 40 mm in length and claddings are removed, before granulation. Then about nine grams of granular fuel is carefully introduced into capsule. The capsule containing the granular fuel is then sealed in a high vacuum of 10"2 to 10-3 Pa by an electron beam welding machine. These preparations are carried out remotely in an alpha-tight steel box(an in-cell box) within a gamma-shielding cell. On this process, the temperature of the whole capsule is liable to rise up by welding heat. It will cause that FP gas retained in the fuel is put away, the pressure in the capsule heightens, the lid of a capsule is pushed up, and then the normal welding becomes impossible. In the worst case, the fuel in the capsule scatters out. Therefore, it is necessary to keep the temperature of the capsule as much as possible low temperature. Then, cooling method of the capsule under welding was devised in this system. In an electron beam welding machine, the tungsten capsule is set by a chuck. The outline drawing of the chuck is shown in Fig. 1. The base design is a three point scroll chuck , and it was improved into the plane chucking system for fitting to the capsular shape. So that the contact area with the capsule drastically increased, and the heat radiation effect was heightened. The chuck is made of copper metal and tantalum liner so that it has also a function of heat sink. The tantalum liner of the high melting point prevents depleting the copper heat sink by heat in a high vacuum condition. In addition, the stainless plate improves the handling by the manipulator is installed in the upper surface of the chuck. The welding process was also devised that the capsule is welded in the low power condition temporary, and complete welding is carried out afterwards.

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DESCRIPTION OF THE MELTING TEMPERATURE APPARATUS

The main part of the apparatus is located in a gamma-shielding cell. Schematic drawing of the apparatus is shown in Fig. 2 and Fig. 3. The furnace unit is installed in an in-cell box. The vacuum chamber is evacuated to lO2 Pa. The specimen, enclosed in a tungsten capsule, is located in a tungsten crucible which is set in the center of the induction furnace to heat up the tungsten capsule uniformly. The water cooled concentrator is equipped to provide the magnetic field with the crucible efficiently and to shield the glass chamber from high temperature radiation. The temperature of the specimen is continuously monitored by two sets of two-color pyrometers. Heating power is controlled by a signal from the upper pyrometer. The temperature of the specimen is monitored with the lower pyrometer sighted on a small diameter well at the bottom of the capsule which simulates black-body. The light path traverses through the revolving protection glass disk, the vacuum enclosure window, and the shielding cell window. The revolving protection glass disk which is nearest to the furnace, prevents the vacuum enclosure window from being coated by vapor deposition. When the protection glass disk is dimmed, the disk is rotated to provide a new clean path.

MAINTENANCE OF THE APPARATUS

On the measurement operation for above 15 years, the capsule occasionally leaked, because of rise of the capsule internal pressure by the volatile FPs, coarsening of crystal grain by the recrystallization of the tungsten and embrittlement being generated in high temperature heating. The volatile FPs which was discharged out under heating deposited to the low temperature portion of the apparatus that is mainly the concentrator in the furnace unit and the exhaust duct of the vacuum pumping system, and the radiation dose rate of the equipment rose very much. The contaminated concentrator can be exchanged periodically, because the remoteness disassembly is possible. However, the exchange is not possible for the exhaust duct, since it is being fixed in the in-cell box. In the point maximum, the dose rate reached 320 mSv/h. Such a high radiation condition interfered with ordinary maintenance of the apparatus. Then, the equipment for the remote decontamination was devised, and the exhaust duct inside and heating furnace inside were tried to decontaminate. However, it was not possible to lower only to about 190 mSv/h, since the inside is very narrow and sufficient decontamination was impossible. Some radiation shielding devices was designed and used for ordinary maintenance such as exchange of the oil of the vacuum pump and exchange of the globe under the environment of such high dose rate. The shielding screen consisted of the lead on 1800 mm height, 1300 mm width, 30 mm thickness. By using these shielding devices, the environment of maintenance area was secured and maintenance of the apparatus was able to be carried out. However, this work is hard to be carried out frequently. Therefore, the whole equipment will be renewed in FY 1999.

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EXPERIMENTAL DATA AND DISCUSSION

1. Accuracy It is most important to obtain the accurate temperature of a specimen in the melting point measurement. It is necessary that absolute temperature is calibrated by the calibration formula in the two-color pyrometer. The temperature reproducibility is high for this pyrometer itself, and the measurement with the high accuracy becomes possible, if the calibration formula is obtained. There is the ratio of observed emissivity to rue one of measured object (i.e., tungsten) as a main error factor of the pyrometer. The emissivity of tungsten is well known, but there are some differences by the surface state (e.g., roughness ). Then, the temperature measuring well was made at the capsule bottom to simulate black-body, in which the effective emissivity was about 1. At first, the well was designed the dimension with 1 mm in diameter and a depth of 10 mm. However, adjusting condition for focusing of the pyrometer is very severe, since a distance from the tungsten capsule is about 2 m and a sight range of the pyrometer is not less than 1 mm in diameter. Then, diameter of the well was enlarged up to 2 mm with the same length that is the limit to get a black-body condition. It contributes to good accuracy of measured temperature data. The uncertainties of measured temperature on each capsule were reduced by this method. Furthermore, transmission of the glass and reflection by the mirror in the measurement optical path affect the emissivity, and it becomes a factor of the indication error. Then it must be corrected as an emissivity ratio. The correction is possible to be carried out by these condition being fixed. However, it must be evaluated at each measurement, since the transmittance of the window glass gradually changes by each measurement operation. At the AGF, melting point of reference sample (i.e., Mo metal of mp 2630*0 and Ta metal of mp 2990^) is measured before and after the measurement of the fuel as an error evaluation method. These reference sample were selected since they are metal sample which melting point is around and near to the fuel's one. As the above description, the slippage of melting point around the measurement of reference sample was adopted as an error of the pyrometer indicating temperature. The whole measurement error is added reading error of thermal arrest in the heating curve. The melting point of unirradiated UO2 was verified being 2845 ± 12*0 at the AGF in which 2847 ± 25'C is the recommendation value of the IAEA [4]. As the other report for unirradiated UO2 using with the encapsulation method, Aitken & Evansns [3], Lyon & Baily [2] and Latta & Fryxell's [5] is representative, and the measurement accuracy is ± 251C, ±2013, ± 15 *C each. These measurement error do not carry out the evaluation of the every sample like this report. For irradiated MOX fuel,Krankota &Craig [6] reported the error ±52^-+ 130'C. This large error was caused by the V-shaped filament method, since the specimen is not enclosing and the composition change is easy to be caused by unequal evaporation and the oxygen transfer. Adamson et al.[7] mentioned about the reliability of the V-shaped filament method that this method gave melting temperatures approximately 50*0 lower than true one.

- 115 - JAERI-Conf 99-009

2.Melting Temperature Data At the AGF, melting temperature has been measured with good accuracy on UO2 and (U, Pu)O2 fuels irradiated in FBRs, ATR, and BWRs. Typical data are shown in Fig.4. The melting temperature of 29 wt% PUO2-UO2 obtained at the AGF are plotted,, comparing with the data of 25 wt% one reported by Krankota and Craig [6]. Their data locate at higher temperature range than the AGF's, and it is well-known that melting temperature decreases with an increase in PuO2 concentration[6,7]. In this data, the maximum burnup of specimen is 124 GWd/t which was irradiated in "JOYO". This figure also includes the data obtained from simulated burnt MOX fuels. They were prepared by adding the non-radioactive oxide powder of eight soluble FP elements to unirradiated or irradiated fuel powder, that amount corresponds to the maximum burnup of 250 GWd/t. These data shows that the melting temperature of 29 wt% PUO2-UO2 decrease almost linearly with burnup at a rate of 5 "C within the lower burnup region up to 170 GWd/t, and almost saturate above it. It may be necessary to measure the actual specimen of higher burnup in order to confirm this behavior.

SUMMARY

A technique and operation for melting temperature measurement of irradiated oxide fuels at the AGF is described. In this technique, the fuel is enclosed in a sealed tungsten capsule to prevent chemical change, and heated in the induction furnace. The melting temperature is determined from arrest of the heating curve. Observed melting temperature of MOX fuel decrease with increasing burnup and saturated at high burnup region.

REFERENCES

[1] For instance; Christensen, J. A., et. al., WCAP-6065 (1965). [2] Lyon, W. L., Baily, W. E., J. Nucl. Mater., 22 (1967) 332. [3] Aitken, E. A., Evans, S. K., GEAP-12229 (1971). [4] M.H.Rand et al., Rev. Int. Hautes Temp. Refract. 15 (1978) 355. [5] R.E.Latta & R.E.Fryxell, J. Nucl. Mater., 35 (1970) 195. [6] Krankota, J. L., Craig, C. N., GEAP-1315 (1969). [7] M.G.Adamson, etal., J. of Nucl. Mater., 130 (1985) 349.

- 116- JAERI-Conf 99-009

Handling plate

Copper heat sink

Tantalum liner

Driving screw

Fig. 1 Structure of the capsule chuck in an electron beam welder

'/7/////7//A cimen (Tungsten capsule) Manipulator ) Heat shielding ) Concentrator • Induction heating coil 1 Vacuum chamber (Quartz) _ Shielding 1 Cooling water window Argon gas supply In-cell box Exhaust duct Hydraulic lift " Gamma-shielding Diffusion pump Rotary pump Mirror Two-color pyrometer Window Induction cable Protecting glass

Inverter

Fig. 2 A schematic drawing of the melting temperature measurement apparatus

- 117- JAERI-Conf 99-009

Specimen Tungsten capsule Tungsten crucible Crucible support • Concentrator • Upper radiation shield Lower radiation shield • Cooling water passage • Isolator (Alumina) • Vacuum chamber (Quartz) • Induction heating coil

Black-body well

Fig. 3 A schematic drawing of the induction furnace unit and a tungsten capsule

Report Pu content (wtS6) Specimen Krankota 3000 O 25 irradiated fuel and Craig A 29 irradiated fuel Data at the AGF • 29 unirradiated fuel+simulated FP 2900 • 29 irradiated fuel+simulated FP

| 2800 8. _|A ..A 2700

2600

2500 L I • I 0 20 40 60 80 100 120 140 160 180 200 220 240

Bunnup (GWd/t)

Fig. 4 Melting temperature of MOX fuels as a function of burnup

118- JP9950633 JAERI-Conf 99-009

2.3 Development of PIE Techniques for Irradiated LWR Pressure Vessel Steels

Masahiro NISHI, Minoru KIZAKI and Tomohide SUKEGAWA

Research Hot Laboratory Division Department of Hot Laboratories Tokai Research Establishment, JAERI Tokai-mura, Naka-gun, Ibaraki-ken, Japan

ABSTRACT

For the evaluation of safety and integrity of light water reactors (LWRs), various post irradiation examinations (PIEs) of reactor pressure vessel (RPV) steels and fuel claddings have been carried out in the Research Hot Laboratory (RHL). In recent years, the instrumented Charpy impact testing machine was remodeled aiming at the improvement of accuracy and reliability. By this remodeling, absorbed energy and other useful information on impact properties can be delivered from the force-displacement curve for the evaluation of neutron irradiation embrittlement behavior of LWR-RPV steels at one-time striking. In addition, two advanced PIE technologies are now under development. One is the remote machining of mechanical test pieces from actual irradiated pressure vessel steels. The other is development of low-cycle and high-cycle fatigue test technology in order to clarify the post-irradiation fatigue characteristics of structural and fuel cladding materials.

1. INTRODUCTION

Mechanical properties of RPV steels and fuel cladding of LWRs at the post irradiation state are the key parameter for the evaluation of safety, structural integrity and lifetime as well as the material development. The mechanical tests at the RHL have been performed for 38 years to support R&D works in this field at JAERI. The data of Charpy impact test are effectively utilized to evaluate the neutron irradiation embrittlement. Recently, the existing Charpy impact testing machine was remodeled in order to improve its accuracy and reliability.

- 119- JAERI-Conf 99-009

By this remodeling, absorbed energy and other useful information can be delivered from one-time striking. In addition, the remote machining technology from actual irradiated RPV steels has been developed in order to clarify the aging behavior of LWRs at the RHL. Another new technique is developed to determine the post-irradiation fatigue characteristics of structural and fuel cladding materials as low and high-cycle fatigue tests technology with the function as tensile test equipment. The present paper describes the outline of two mechanical testing apparatuses and techniques and remote machining of mechanical test pieces for irradiated LWR-RPV steels and so on.

2. REMODELING OF CHARPY IMPACT TESTING MACHINE

2.1 Remodeling The Charpy impact testing machine was redesigned and modified in order to clarify the neutron irradiation embrittlement behavior of LWR-RPV. This machine instrumented with electronic measuring devices to detect an impact force and a displacement of specimen has an automatic specimen setting system. The block diagram of instrumented Charpy impact testing machine is shown in Fig.l. The load capacity is 300J and it is possible to test in the

•DISPLACEMENT MEASURING SYSTEM- FORCE MEASURING SYSTEM

HAMMER (SEMICONDUCTOR ACTIVE STRAIN GAGES)

Fig.l Block diagram of instrumented Charpy impact testing machine

- 120- JAERI-Conf 99-009 temperature range from -140t to 240°C by using two types of agitated liquid baths. The test specimen is transferred from the cooling (or heating) bath to an anvil of the machine using industrial robot, and struck by a hammer within 4 seconds after removal it from the medium. The test temperature accuracy is within 0.5^. The test items are V-notch Charpy impact test and KId dynamic fracture toughness test. The data from Charpy impact test are evaluated on ductile/brittle transition temperature using least squares method, referring a polynomial expression, a hyperbolic tangent and a Gaussian error function. The sensor for the load detection was composed of two semiconductor active strain gages on the tup and two dummy gages put on near the hammer. Moreover, a potentiometer for the displacement detection was inserted and fixed to the hammer shaft. These signals from sensors are recorded in the wave-memory with the capacity of 32Kwords x 2 channels, the resolution of 12bit and the sampling rate of 50~500nsec/word. Collected data are utilized for data processing and analysis.

2.2 Characteristics A calibration technique is most important in the instrumentation, because it is utilized to convert the data sampled by measuring devices to the force and displacement. The calibration must be carried out in a constant condition that is never affected by a human error and the environment. The RHL developed completely new methods for a load calibration technique as shown in Fig.2. The calibrator can be fastened with positioning and height adjusting to the specimen support on anvils without causing pre-strain to the semiconductor gages pasted on the hammer tup. Therefore, the calibration is possible by the comparison between a proof load from the calibrator and an output of the force- measuring device. In addition, the RHL found that the conversion value should be corrected every time because an output mentioned above changes with a change in ambient temperature. An equation of correction derived from proof tests offers a high accurate conversion value. On the other hand, the calibration method for the displacement measurement is shown in Fig.3. For the same reason, the calibrator with an electric micrometer is also fixed to the specimen support. Then, calibration is performed by comparing a proof displacement from the calibrator with an output of the displacement-measuring device.

2.3 Performance An example of obtained data from PIE is shown in Fig.4. A force- displacement curve shows the impact properties during the striking very clearly. The Fgy, Fm, Fu and Fa marked on the curve mean a yield impact force, a maximum impact force, an unstable crack (cleavage crack) initiation force and a crack arrest force respectively. While, the Einst is total impact energy which is

- 121- JAERI-Conf 99-009 area under the complete force-displacement curve. In addition, the curve offers a ductile erack initiation energy, partial impact energy at above points, total displacement of specimen and so on. These impact properties and characteristic values of the points are defined in accordance with ISO standard ISO/DIS 14556(1). As shown in the figure, the Fgy, Fm and Fu decrease with increasing the test temperature, whereas the Fa increases. The Fa on the curve means a specimen struck in the transition range. The force-displacement curves obtained from PIE after remodeling are very useful data for the evaluation of irradiation embrittlement.

SIGNAL FROM CSEMICONDUCTOR STRAIN GAGE

PROOF LOAD APPLYING SYSTEM (0~3ton)

Fig. 2 Force cal ibrator

0 MOVED AXIS ANGLE

SIGNAL FROM POTENTIOMETER J—»\AMPLIFIERJ

HAMMER ELECTRICAL MICROMETER

TUP WITH SEMICONDUCTOR STRAIN GAGE'

ilSPLACEMENTOnm) Fig. 3 Displacement calibrator

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Material: A533B-1 Fluonce: ~9X1O" n/cm2 Fm(Fu) Fm Fm Curves CD ® <3) ® Test Temp (°C) 50 120 125 180 Shear Area (%) 7 37 71 100 (KN) 16.028 15.891 15.823 15.469 Fgy (mm) 0.442 0.436 0.438 0.452 (kN) 18.679 18.970 18.795 18.061 (mm) 0.936 1.715 1.898 1.687 (kN) 18.679 18.579 17.103 — Pi • (mm) 0.936 1.849 3.187 —

Fa (kN) — 7.246 9.763 — (mm) — 1.950 3.192 -

Displacement

Fig.4 An example of PIE data obtained from remodeled Charpy impact testing machine

3. DEVELOPMENT OF REMOTE MACHINING TECHNOLOGY

3.1 Design concept In case of irradiated material, since all of manipulation must be remotely handled, machining of the mechanical test specimen should be performed accurately in accordance with the material testing standards such as ISO, ASTM and JIS. However, the remote machining with high accuracy has never been done up to date because the requirement is quite difficult. Therefore, a numerically controlled machine tool is selected and developed as the most useful apparatus for hot cell work without a human error. As shown in Fig.5, a computerized numerical control (CNC) milling machine developed is composed with the main body for machining and a control system included a personal computer. There are two main bodies produced by same design, which can be operated by an identical controller. One is installed in the hot cell and the other is set up in the operating area for mock-up test prior to in-cell machining. The original machine for general use is modified according to some requirements from radiation environment, free maintenance and higher

- 123- JAERI-Conf 99-009 performance. Moreover, the innovational techniques are applied to achieve the allowable machining by means of remote handling.

Fig.5 Computerized numerical control (CNC) milling machine

Fig.6 Charpy (type-A) impact test specimen machined by CNC milling machine

3.2 Characteristics and Specification The CNC milling machine developed is extremely compact of 850 x 800 x 1100mm and quite on a par with a general machine tool in mechanical accuracy. In addition, the main body with an automatic tool changer (ATC) included necessary six tools is highly rigid portal structure. The parts reviewed and redesigned are as follows. The motor for X/Y/Z motion was modified from a DC servomotor with rotary encoder to an AC servomotor with resolver. DC servo

- 124 JAERI-Conf 99-009 spindle motor of 200w was also changed to an AC servo of 800w. Then, a magnetic device was selected as the sensors for positioning and the amplifiers were located into control box in operating area. Moreover, the innovational techniques added are as follows.

3.2.1 Clamping mechanism of the work A clamping mechanism is composed with a hydraulic vise for clamping of a four-cornered work and an electric rotating chuck with AC servo resolver motor combined a bearing which is able to rotate the vice. Therefore, it is possible to machine without re-clamping on five surfaces except bottom of the rectangular work and notch-machining to the top surface.

3.2.2 Automatic measuring mechanism of the origin in Z-motion In case of a general machine, the origin of Z-motion is manually decided by using a so-called touch sensor, standard gage, which can indicate a contact point of the mill tip and the sensor top. However, decision of the Z-origin with remote handling is not so easy because the largish sensor must be set on a central part of the smallish work. For that reason, the automatic measuring mechanism that is able to detect a contact point through an electrical signal was designed. This idea was accomplished by insulating of spindle using a ceramic coating.

3.2.3 Machining techniques In general, the tool and work during machining is cooled by plenty of oil, however, the dry machining is the best way, in case of hot cell work, if possible. CNC milling machine in the RHL has an air-cooling system and an intermittent oil-atomizer, which performs the duty as a lubricant rather than a coolant. The dry machining is achieved by finding out the suitable conditions including kind of machining, selection of tool, machinability of work, cutting and feed speed and so on. Then, an atomizer automatically and periodically sprays cutting oil, if it is necessary. One of problems in specimen machining of RPV steels is the removing technique of barr (frash) growing on edges. To resolve the problem, the unique mechanism that is utilized CNC milling function is now under development. By this idea, the barr will be removed by a whetstone with automatic operation as a series work of the machining.

3.2.4 Automatic marking technique for identification To avoid a blunder, the marking for identification should be performed during the machining or immediately after it finished. In addition, the marking must not affect mechanical and metallurgical properties of the specimen. Automatic marking of identification number is possible by combining a

- 125 JAERI-Conf 99-009 pneumatic marking pen with a function of CNC milling machine. The pen is fixed by air chucking with easy handling like a machining tool on ATC magazine. Therefore, the identification number can be automatically marked on the programmed position according to command with key-in.

3.2.5 Dimension measuring system for the machined specimen The machining error that is the deviation from programmed nominal value is mainly depending on the rigidity and actual diameter of the tool. To compensate the error, the CNC operation program requires the difference between the command and as-machined condition. Therefore, a dimension measuring system utilized CNC milling function was designed. It is composed with two SONY magnescales for measuring the X/Y motions, a touch sensor for commanding the start/end of measuring, a display unit (counter), a resetting jig of the sensor and a holder for combining the sensor with CNC milling body. The sensor is able to touch automatically one side surface and the opposite face of the machined specimen and measures the wide and length. In addition, the TV monitoring system for confirming the machined notch- shape is now under investigation.

3.3 Performance The machining programs developed in the RHL are a Charpy impact test specimen type A of 10 x 10 x 55(mm) so-called V-Charpy, a plate type tensile test specimen with parallel part of 22.95Lx 3Wx 3t(mm), and a three point bending type fracture toughness test specimen with knife-edges. The CNC milling machine is possible to machine these specimens with high accuracy that satisfies the standards, ISO, ASTM and JIS. As one of examples, a machined Charpy impact specimen is shown in Fig.6. For checking of the machining condition, there are a sound sensor and an acceleration sensor on the body. Moreover, a TV monitoring system for observing of tool-edge chipping and chips of work is located nearby the machine.

4. DEVELOPMENT OF REMOTE SYSTEM TECHNOLOGY FOR FATIGUE TESTING

4.1 Fatigue testing machine One of the important research subjects on the LWR fuel cladding performance at extending burn-up is to understand the mechanical properties. The RHL developed an electro-hydraulic fatigue testing machine with two kinds of load cells and servo valves in tandem and in parallel respectively.

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Main load cell with 20KN is used when the maximum load will be more than 2KN for dynamic and 3KN for static loads. Sub load cell with 2KN is utilized for the specimens with lower maximum load than the above-mentioned one. In case of servo valves, the larger valve with discharge rate of 38 1/min is utilized for the high frequency test condition with high load. It is possible to load up to lOOHz. The smaller one with discharge rate of 3.8 1/min is very useful for most of PIEs such as a low frequency test, a lower load test and all of static tests. Therefore, even the tension/compression tests bellow 200N, it is possible with high accuracy. A changing of the signal between the larger ones and the smaller ones can be carried out by manual work at in-cell for the load cells and by switching from out-cell for the servo valves. By exchanging the test fixtures with remote handling, the machine is utilized for a high-cycle fatigue test with arc-shaped specimen machined from LWR fuel cladding, a low-cycle fatigue test with round specimen from structural materials, a crack propagation test and a high-frequency test. Moreover, tensile test, plan strain fracture toughness test and the fatigue pre-cracking for fracture toughness specimen are also possible. The specification and the performance of fatigue testing machine are shown in Table.1.

4.2 Characteristics The alignment of load train including a specimen is the most important in the fatigue test. ASTM standard (2) recommends that the bending moment during the full-reverse testing should be maintained within 5% of axial load. This is not so easy even a general test. The developed fixturing technique is able to make sure the allowable alignment every time with easy operation in spite of remote handling using manipulators. The fixturing way for the RHL fatigue testing machine is as follows. In case of a arc-shaped specimen with parallel part of 2.5w x 5L x 0.7t (mm) that has very poor rigidity, the specimen is fastened with volts to upper and lower test fixtures by means of an assembling device which is able to tighten uniformly and constantly with easy operation using manipulators. The upper and lower fixtures connected and reinforced by the support handle are placed into the sockets of pull rods. Finally, both fixtures are held by the hydraulic clamping system. Because of that, the specimen can be fixed without a significant pre-strain. On the other hand, a round type specimen with parallel part of

- 127 - JAERI-Conf 99-009 fatigue test can be hold within 5% of the axial load. Gripping and setting for the static tests are also conducted easily by similar method. The excellent alignment can be readjusted by using an alignment measuring system, which consists of a verification bar with four strain-sensing devices, a display and analysis apparatus for local strains. And the adjusting can be carried out with cautions of handling and with monitoring the rectangular coordinates chart on CRT in real time, which indicates the four local strains on the bar during the handling.

Table.1 Specification and performance of fatigue testing machine © Type of machine Fatigue testing machine equipped with electro-hydraulic servo actuator SHIHADZU EHF-ED20KN-20LA © Capacity Load frame ; ±100KN(dynamic load) dynamic load , static load ® Performance Main load eel I ±20KN , ±30KN for high-load Sub load eel I ±2KN , ±3KN for low-load Load range ±0. 2 to 20KN, ±0.2 to 30KN Frequency range 10"5~102 Hz Actuator speed 1 .56x10"5~103 mm/sec 7 2 6. 25X1O" ~6X1O KN/sec © UtiIization Tension/compression tests as follows, for mechanical tests Fatigue test (full-reverse); High-cycle and low-cycle fatigue tests crack propagation test and high frequency test Static test ; Tensile & plan strain fracture toughness tests (unloading compliance method) for preparation work Fatigue pre-cracking for fracture toughness specimen © Test conditions Temperature; -140~450°C in temperature chamber Atmosphere ; air Alignment ; Bending strain during the full-reverse fatigue test is within 5% of axial strain Specimen Round specimen with button head connection(standard) for fat igue test OveralI length ; 44 mm Parallel part ;#4x8 mm , G.L 6 mm Shoulder radius °. R15.6mm Arc-shaped specimen taken from LWR fuel cladding Total length ; 40mm Parallel part ; 2.5WX5LX0.7T mm for tensi le tests Round specimen ; PP. #4x 22.0L55 mm Arc-shaped specimen; PP.2.5WX15Lx0.7T.OL40 mm PP(parallel part) for fracture CT type ; 0.4CT, 0.5CT, 0.63CT toughness test DCT type ; 0.4DCT, 0.5DCT, 0.63DCT pre-cracki ng 3-points bending fracture toughness specimen

4.3 Performance In case of an arc-shaped specimen, the fastening torque of 10.3 N-m for inside volts and 39.2 N-m for outside volts makes suitable test condition. These values obtained from experiments are accurately controlled every time by using the torque meter with strain gage. With regard to the cycle frequency, it is possible to utilize up to 40Hz. This is good performance, because even a test up to 107 cycles, it is achieved only within 3 days. Fig.7 shows a plot of data from the RHL machine and from a literature(3) on unirradiated Zry-2 specimen. Test

- 128- JAERI-Conf 99-009 was performed with cycling frequencies of 3 to 40 Hz and with a stress ratio of R~°min// °max= ~~ 1 at room temperature, and loading stress of ±164 to +492 Mpa with sine wave. As shown in figure, the fatigue lives from the RHL machine agree with the reference values which were taken by the standard testing method, in spite of an arc-shaped cross section of an imperfect symmetry. On the other hand, the low-cycle fatigue test results with a 4 round specimen of Hastelloy XR- II agree quite well with the conventional test specimen of parallel part of $ 10 x 20L(mm) .

1.00E+06

1.00E+O5

A • (

Ul CM 1.00E+04 A REFERENCE(3) • THIS WORK

1.00E+02 1.00E+03 1.00E+O4 1.00E+O5 1.00E+06 1.00E-KI7 CYCLES TO FAILURE . N

Fig.7 Fatigue data on unirradiated Zry-2 (at room temp.)

5. CONCLUSION

By remodeling of Charpy impact testing machine, absorbed energy and other useful information on impact properties can be delivered from the force- displacement curve for the evaluation of neutron irradiation embrittlement behavior of LWR-RPV steels at only one blow of a hammer. Development of the CNC milling machine makes possible not only machining of mechanical test specimens from actually irradiated structural materials but also converting the Charpy V-specimen irradiated into a fracture toughness specimen. The establishment of this technique with fatigue pre- cracking will contribute to more precise life evaluation of RPV steels in LWRs

- 129 - JAERI-Conf 99-009 by utilizing the surveillance specimen. With regard to development of the fatigue testing technology, it was proved that developed fatigue testing machine and its technique offer the valid results in high-cycle and low-cycle fatigue tests with full-reverse loading. The high-cycle test technique developed will be utilized to evaluate the fatigue property in high-burnup program for LWR fuel in near future. The low-cycle test technique using a round specimen is the most useful and will be used in R&D works of the structural materials for the future.

6. ACKNOWLEDGMENTS

The authors acknowledge to Dr. T Kodaira, director of Department of Hot Laboratories, for his valuable advice. The authors would also like to thank to the staffs of the RHL for their assistance in performing the experiments.

7. REFERENCES (1) INTERNATIONAL STANDARD ISO/DIS 14556(draft) Steel-Charpy V-notch impact test-Instrumented test method, (1998) (2) ASTM Designation: E606-92 Standard Practice for Strain-Controlled Fatigue Testing, (1996) (3) W.J.O'Donnell and B.F.Langer: Fatigue Design Basis for Zircaloy Components, NUCLEAR SCIENCE AND ENGNEERING, 20,1-12(1964)

- 130 - JP9950634 JAERI-Conf 99-009

2.4 HIGH RESOLUTION GRAIN BOUNDARY ANALYSIS OF NEUTRON IRRADIATED STAINLESS STEEL USING FEG-TEM

Mitsuhiro Kodama, Yoshihide Ishiyama and Norikatsu Yokota Nippon Nuclear Fuel Development Co., Ltd.

ABSTRACT

High-resolution grain boundary analyses of irradiated SUS304 stainless steel using a field emission gun equipped transmission electron microscope were carried out in order to detect radiation-induced grain boundary segregation. The effect of probe size on the measured compositional profiles was studied. The depletion of chromium and enrichment of nickel, phosphorus and silicon were detected at a grain boundary. The measured compositional profiles were affected by the probe size which impeded their interpretation.

INTRODUCTION

Radiation-induced segregation (RIS) is as one of the radiation-induced phenomena which are closely related to the point defects introduced by irradiation. Recently, RIS in the vicinity of the grain boundary has attracted interest, because of its possible significant effect upon chemical and/or mechanical properties of the austenitic stainless steels which are used as light water reactor core components [1,2].

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A number of studies using a conventional transmission electron microscope (TEM) [3-6] have appeared about RIS in stainless steels irradiated by ions or electrons. However, conventional TEM measurements of RIS profiles across the grain boundary in stainless steels neutron-irradiated in power reactors are difficult to make because the segregated zone in these steels is very narrow (a few nanometers) due to the low irradiation temperature (about 300*0). The recent development of the field emission gun (FEG) makes it possible for TEM analysis to treat regions as small as lnm or less, while a conventional TEM analyzes a ten times larger region. For localized changes in concentration induced by neutron irradiation at the grain boundary in austenitic stainless steels, the FEG is required to provide electron probes with small diameter (~lnm) and sufficient current to allow X-ray measurements. In this paper, grain boundary analyses of SUS 304 stainless steel irradiated in a LWR plant using FEG equipped TEM (FEG-TEM) were carried out in order to detect RIS at a grain boundary. The effect of the probe size in the energy- dispersive X-ray spectrometer (EDS) analysis of measured compositional profiles was also examined.

EXPERIMENTAL PROCEDURE

1. Materials Solution-treated SUS 304 stainless steel obtained from an operating LWR plant was used. Chemical composition is listed in Table 1. This steel was neutron irradiated in the mid-core region. Neutron fluence was 2.0xl025n/m2 (E>lMeV). Nominal irradiation temperature was 561K.

2. Analysis TEM analysis samples were machined to coupons and mechanically ground to reduce their thickness to 0.1mm. Disks of 3mm diameter were punched out and from them, lmm-diameter disks were punched out to reduce the volume and to

- 132- JAERI-Conf 99-009 minimize radiation flooding of the X-ray detector. Each disk was pressed into a lmm diameter hole of an "unirradiated" annulus to form a composite as shown in Fig. 1. The composite was electropolished in a twin jet Tenupol unit. The electrolyte consisted 95% acetic acid and 5% perchloric acid. This technique could reduce the intensity of radioactivity of an irradiated TEM specimen to below 10% of its original value. Elemental compositions across grain boundaries were measured by EDS using a Hitachi HF-2000 FEG-TEM. A large angle grain boundary was selected for examination. Analyses were performed on the grain boundary and at points 1, 2, 3, 4, 5, 10 and 20nm on either side. X-ray counts were carried out for 100s periods, with readjustment of the beam position when necessary. X-ray counts were converted to chemical compositions using the Cliff-Lorimer approximation [7]. The compositional analyses were performed using 1 and 2nm incident electron probe sizes.

RESULTS AND DISCUSSION

Compositional profiles across a grain boundary with two different probe sizes are shown in Fig. 2 for SUS304 stainless steel irradiated to 2.0xl025n/m2 (E>lMeV). The depletion of chromium and enrichment of nickel, phosphorus and silicon were detected at the grain boundary. The profiles measured by the two probe sizes agreed qualitatively. However, for results by the lnm probe, segregation at the grain boundary was high and the width of segregated zone was narrow compared with results by the 2nm probe. These data indicated that the measured compositional profiles depended on the probe size. The theoretical prediction of RIS was obtained by a computer simulation [8], for comparison with the experimental results. The line in Fig. 3 shows the theoretical chromium profile across a grain boundary. The calculated width and concentration at the grain boundary were not in agreement with the measured ones. From these data, it was expected that the width of the actual segregated zone was very narrow compared with the measured one.

- 133 - JAERI-Conf 99-009

Using FEG-TEM at present, the atomic scale concentration change cannot be directly detected in a local region by EDS because the nanometer probe at a sample surface still encircles several atoms or atomic columns. This fact implies that what is acquired as a local profile of the specimen in the EDS analysis is spatially averaged information about the actual composition profile. Thus, in order to evaluate the effect of the probe size in the EDS analysis on measured compositional profiles, the measured compositional profile changes were predicted by averaging the calculated compositional profile at two probe sizes. The detail averaging method was described in the literature [8]. Fig. 4 shows the effect of the probe size on the average. As could be expected, the averaged compositional profiles were blunted near the grain boundary and broadened as the probe size increased. Predicted and measured chromium profiles are shown in Fig. 5. When the effect of the probe size was considered, good agreement was obtained between predicted and measured compositional profiles. These results suggested that considering the effect of the probe size was needed when narrow compositional profiles were measured by EDS.

CONCLUSIONS

(1) Radiation induced grain boundary segregation (the depletion of chromium, and enrichment of nickel, phosphorus and silicon) was detected using FE-TEM in SUS304 stainless steel neutron-irradiated at low temperature. (2) Analysis results for the lnm probe showed the segregation at a grain boundary was high and the width of the segregated zone was narrow compared with results for the 2nm probe. (3) Narrow compositional profiles measured using EDS were affected by the probe size. The effect of probe size on the measured compositional profiles was judged to be important.

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REFERENCES 1. PL. Andresen et al., Proc. of 4th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems-Water Reactors, Jekyll Island, Georgia, August 6-10, (1989), p.83. 2. K. Fukuya et al., Proc. of 6th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems-Water Reactors, San Diego, California, August 1-5, (1993), p.565. 3. N.Q. Lam and P.R. Okamoto, ASTM Spec. Tech. Publ. No.870 (1985) p.430. 4. K. Nakata and I. Masaoka, J. Nucl. Mater., 150 (1987) p.186. 5. K. Fukuya, et al., J. Nucl. Mater., 179-181 (1991) p. 1057. 6. T. Kato, et al., J. Nucl. Mater., 189 (1992) p.167. 7. G. Cliff and G.W Lorimer, J. Microscopy, 103 (1975) p.203. 8. S. Watanabe et al., J. Nucl.Mater., 224 (1995) p.158.

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Table 1 Chemical composition (wt%

Steel C Si Mn P S Ni Cr Fe Type 304 0.05 0.51 1.69 0.029 0.007 10.2 18.65 bal.

Irradiated

Unirradiated

3mm" I+ Electropolished Observation area

Fig. 1 A schematic illustration of the preparation of a TEM specimen

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23 • Probe size:1nm 16 • Probe size.'Iran • Probe size:2nm • H Probe size:2nm 22 • 14 > 21 ?20 • 12 J I • ma 19 o • 2 10 18 • 8 17 4

. . . m . . . m . . . . -15 -10 -5 0 5 10 15 -15 -10 -5 0 5 10 15 Distance from G.B. (nm) Distance from G.B. (nm)

• Probe size:1nn 3.0 0.5 Probe size:1nm • Probe size:2n•n Probe size:2nm 2.5 1 0.4 ; *» 2.0 m1 •0.3 1.5 •* • C/) Q.0.2 1.0 • • • 0.1 0.5 *• • " . . - ...... 0.0 -15 -10 -5 0 5 10 15 -15 -10 -5 0 5 10 15 Distance from G.B. (nm) Distance from G.B. (nm)

Fig. 2 Compositional profiles of a grain boundary in SUS 304 stainless steel irradiated to 2.0xl025n/m2 (E>lMeV).

- 137- JAERI-Conf 99-009

nc G.B. • Probe size:1 nm • Probe size:2nm # k 20

J] Theoretical 15 t calculation o 10 : I •

-15 -10 -5 0 5 10 15 Distance from G.B. (nm)

Fig. 3 Comparison of the experimental results and the theoretical chromium profile across a grain boundary.

G.B. 25 i

20 I 2nm 15 s 1nm o

10 As calculated'

-10 -5 0 5 10 Distance from G.B. (nm)

Fig. 4 Measured concentration profile changes predicted by averaging the calculated concentration profile for two probe sizes.

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G.B. 23 (a) • probe :1 nm 22 •• • • 21 • • • 20 \ t 19 o 18 V 17 I 1 16

in . • • . . • . . . • • . -15 -10 -5 0 5 10 15 -15 -10 -5 0 5 10 15 Distance from G.B. (nm) Distance from G.B. (nm)

Fig. 5 Comparison of measured chromium profiles with predicted ones. The lines are the profiles predicted by averaging for (a) lnm and (b) 2nm probe sizes.

- 139 - JAERI-Conf 99-009 JP9950635

2.5 The Development of Crack Measurement System Using the Direct Current Potential Drop Method for Use in the Hot Cell

Dosik, KIM, Sangbok, AHN and Key-soon, LEE

Korea Atomic Energy Research Institute, Irradiated Materials Examination Facility P. O. Box 105, Yusong, Korea, 305-600

Yongsuk, KIM and Sangchul, KWON

Korea Atomic Energy Research Institute, Zirconium Development Department P. O. Box 105, Yusong, Korea, 305-600

ABSTRACT

The crack length measurement system using the direct current potential drop (DCPD) method was developed for the detection of crack growth initiation and subsequent crack growth. The experimental precautions and data processing procedure required for its application were also described and discussed. The system presented herein was specially built for use in fracture toughness testing of unirradiated or irradiated pressure tube materials from nuclear reactor. The application of this system for fracture toughness determination was illustrated from the test of curved compact tension specimens removed from CANDU reactor pressure tubes. The crack extension was monitored using the DCPD method. It is found that the changes of the potential drop and the changes of the crack length have a linear relationship. The final crack front was marked by heat-tinting after the test and the specimen broken open for determination of the initial and final physical crack length. The physical crack lengths, obtained by the 9-point average method described in ASTM El737-96 on heat-tinted fracture surface, were used to calibrate the DCPD method for each test on an individual basis by matching the change in voltage to the crack extension. It is found that this system can be recommended for determination of the 7-integral resistance (J-R) curve of unirradiated or

- 140 - JAERI-Conf 99-009 irradiated materials in the hot cell, especially when testing at elevated temperature and in the environment chamber or furnace.

INTRODUCTION

Precise measurements of crack extension are crucial for the determination of reliable fracture toughness and fatigue crack growth rates. Various crack measurement techniques have been applied, including optical (visual and photographic), ultrasonic, acoustic emission, electrical (eddy current and potential difference), and compliance (COD and back face strain gages) methods. Optical, compliance and electrical potential difference are the most common laboratory techniques. The optical technique [1] is simple and inexpensive, and calibration is not required. Accurate measurements can be performed provided the specimen is carefully polished and does not oxidize or corrode during the test. However, crack length is usually underestimated with this method. The process is time consuming and can be automated only with complicated and expensive video-digitizing equipment. In addition, many fracture mechanics tests are conducted in simulated-service environments that obscure direct observation of the crack. The trend toward laboratory automation has resulted in the development of indirect methods of determining crack extension, such as specimen compliance and electric potential difference monitoring. The methods used to measure changes in compliance [1-3] include crack-opening displacement (COD), back-face strain, and crack-tip strain measurements. Among those, the COD method is less expensive, the specimen need not be visually accessible, and it provides an average crack length figure where crack-front curvature occurs. Also, it can be used as a remote method and is easily automated. However, the COD technique has its limitations: it is use for specimens where time-dependent, time-independent, and reversed plasticity effects are small, and has difficulty in attaching clip gage to small specimens in environmental chambers or furnaces. On the other hand, the electric potential difference (EPD) methods are applicable to virtually any electrically conducting material in room-temperature applications as well as high-temperature applications. It can be used for detecting crack initiation and measuring crack growth in the laboratory. Both direct current (DC) and alternating current (AC) techniques have been used to measure crack size in test specimen. For the more common direct current potential drop (DCPD) technique [4 —10], it is simple, robust, and of relatively low cost. This method is amenable to automation and for long-term high-temperature testing but is well established for only certain specimen geometry. However, the method has the limitation of not distinguishing between the crack extension and external dimensional changes

- 141 - JAERI-Conf 99-009 of the specimen that would typically occur during general yielding and is not suitable for large specimens. Its application is totally dependent on an accurate calibration relating output voltage to crack length. This study describes the development and application of a direct current potential method of crack length monitoring for use in fracture toughness testing in the hot cell. The crack length measured by DCPD method is compared with the observed crack length on the specimen surface. And this system is verified through the /-integral test using curved compact tension (CCT) specimen removed from the CANDU pressure tube.

FRACTURE TOUGHNESS TESTING SYSTEM

The elastic-plastic fracture toughness, 7-integral, test procedure requires simultaneous and continuous measurement of load, load-line displacement and crack length during the test. The direct current potential drop (DCPD) technique is a widely accepted method of monitoring crack initiation and growth in controlled laboratory tests. In its simplest form it involves passing a constant current through the test piece and accurately measuring the electrical potential across the crack plane. As the crack propagates, the measured potential drop (PD) increases due to the reduction in uncracked sectional area of the test piece. Typical apparatus for the DCPD technique is illustrated in Figure 1. The basic equipment for the DCPD method consists of a source of constant dc current, a voltmeter of measuring the potential differences that are produced across the crack plane and DCPD IEEE reversing current unit. A very stable source of constant electrical current is required to maximize the sensitivity of the apparatus. HWD 20-10 Transistorized Regulated Power supply manufactured by Mid- Eastern Industries, Inc. was used to supply a constant DC current to the specimen. This supply can be set to any current between 0 to 10A with excellent long-term stability and very low noise levels. The voltage measuring circuit was required to measure continuously changes of the order of microvolts in a signal of several millivolts. Initially, the potential leads were connected to a Hewlett-Packard 3457A multimeter with 6.5digits of resolution. EPD data was taken in the following procedures. A digital pulse from the INSTRON 8500 Plus occurs at the maximum load. This pulse then triggers the Hewlett-Packard multimeter to capture data. Using a small area (20%) allow the EPD voltage to be captured at the maximum load. Maximum load corresponds to maximum crack opening and gives the best resolution for crack length determination during test. In addition, for improving voltage measurement precision, voltage lead wires were twisted and were held to reduce stray voltage induced by changing magnetic fields. Grounding of all devices (current supply, voltmeter, and so on) was

- 142 - JAERI-Conf 99-009 made properly. For DCPD system the thermoelectric effect was taken into account by measuring voltage while reversing the direction of current flow [11]. Testing was conducted on INSTRON 8500 Plus hydraulic testing machine. The pull rods and the grips are machined from heat-treated steel. Test fixture for 7-integral tests was electrically insulated from the test machine to prevent short-circuiting of the DCPD apparatus used for crack extension measurement. This can be achieved by making and inserting the Teflon insulation plates between the test fixture and load cell and actuator. Load-point displacement was measured continuously by the two linear variable differential transducer (LVDT) attached at the both load-line of the CCT specimen during the 7-integral test, Figure 2. The elastic displacement of the load train was excluded by using the LVDT signal [12, 13]. The average value of the corrected LVDT readings is taken as the load-line displacement for calculating 7-integral.

MATERIAL AND TEST PROCEDURES

Zr-2.5%Nb CANDU pressure tube materials were tested in this study. The inside diameter and nominal wall thickness of the pressure tube were 103mm and 4.3mm, respectively. The specimen used in 7-integral fracture toughness tests was cut from CANDU pressure tube by electric discharge machining. The dimensions of specimens are shown in Figure 3. Except for the thickness and the curvature of the tube, the in-plane dimensions of curved compact tension (CCT) specimen are in the proportions described for compact tension specimen in ASTM Standard Test Method El737-96 for 7-integral Characterization of Fracture Toughness [14]. For the measurements of crack extension during 7-integral test, the DC current leads were asbestos-covered nickel-copper wire, 2.1mm in diameter, screwed into the appropriate places of specimen allowing 6A to be carried. The voltage measuring leads were nickel-copper wires, 0.6mm in diameter, spot-welded to opposite side within lmm of the crack mouth as shown in Figure 4. Before 7-integral testing, the CCT specimens were fatigue-precracked for about 4.76mm at room temperature so that the final crack depth (a/W) was about 0.53, where a is the crack length and W is the width of specimen. The initial maximum stress intensity factor and the final maximum stress intensity factor were about 16.3 and 12.7MPa mm, respectively. The fatigue precracking was performed with sinusoidal waveform having stress ratio (minimum to maximum load ratio, R) of 0.1. The tapered loading pins with 1.5degrees of taper were used for producing straighter fatigue precrack. In order to monitor the fatigue crack growth, at first a small area on surface of the specimen ahead of the crack tip was polished, and then the

- 143- JAERI-Conf 99-009 crack growth was observed with a magnifying (X80) travelling microscope. The /-integral tests were performed in air using a constant displacement rate of 0.25mm/min. The crack extension was measured by DCPD method. The tests continued until the PD indicated that the crack had propagated for about 3 to 4mm. After completing the final loading, the area of slow-stable crack extension at the end of the test was heat-tinted for 30minutes at 300°C and observed by optical measuring microscope. The initial and final crack lengths were measured by the ASTM El737-96 nine-point average method. The ratio of the total change in crack length to the total change in PD was used to interpolate the crack length during the test, assuming a linear relationship. The J-R curve was then calculated using ASTM Test Standard E 1737-96.

RESULTS and DISCUSSION

The DCPD technique relies on the relationship between the crack length and the measured potential, which can be determined either by empirical or theoretical means. The typical closed form expressions of a voltage versus crack length relationship that applies approximately for the CT specimen geometry is given in ASTM El737-96 and E647-95a [15]. However, if wire placement (current or voltage) or testing environment has been altered, the suggested relationship is no longer valid, and a new relationship must be developed. Some researchers have used the saw-cut method to obtain the calibration curve [4]. In practice, the possibility of short circuits across the crack opening exists, especially due to the roughness of the fracture surface. Also, there could be some problems to apply the saw-cut method to the irradiated materials. Alternatively, we have observed optically the crack length on the specimen surface. Although the optical surface measurements can not give an average crack length along the crack front, the relationship between the crack length and the potential drop can be obtained. The fatigue crack growth was monitored by polishing a small area on surface of the specimen ahead of the crack tip and by observing the crack growth with a magnifying (X80) travelling microscope as shown in Figure 5. Figure 6 shows the crack length monitored on the specimen surface by a magnifying (X80) travelling microscope with PD signals measured during the fatigue crack growth test for CCT specimen at room temperature. As expected, the crack length is linearly increased with an increase in PD. We found the linear relationship between the crack length and the PD. But, the proportional factor determined in Fig. 6 can not be used to established the J-R curve because of the effects of the plasticity on the measured potential during the /-integral test. Therefore, we assumed that the change of potential drop was proportional to the change of crack length. Then the

- 144 - JAERI-Conf 99-009 proportional factors were obtained for each specimen by measuring the total potential change during the test and the total stable crack growth. The total stable crack length was measured by the nine-point average method in ASTM El737-96 on the heat-tinted fracture surface after the test. A typical heat-tinted fracture surface is shown in Figure 7, in which three regions can be observed. The fatigue crack fronts were usually quite straight, indicating that the curvature of the curved specimen did not change the stress distribution significantly. The stable crack had a thumbnail shape, which is quite symmetric with respect to the thickness of the specimen, indicating again that the curvature did not modify the stress field near the crack tip significantly. A computer program was developed to generate the J-R curve using the procedures described in earlier. Typical J-R curve of unirradiated CANDU pressure tube at room temperature is given in Figure 8.

CONCLUSIONS

(1) The DCPD system developed in KAERI has been successfully used to measure the crack length of curved compact tension specimen in the hot cell. (2) A quite straight fatigue crack and stable crack fronts were obtained on the fracture surface of curved compact tension specimen by using the 1.5° tapered pin. (3) Assuming the linear relationship between the changes of potential drop and the changes of crack length measured by nine-point average method and using computer program developed in this study, J-R curve can be established.

REFERENCES

1. Richards, C. E., "The Measurement of Crack Length and Shape during Fracture and Fatigue," Beevers, C. J., Ed., Engineering Materials Advisory Services, Warley, U.K., (1980) pp.461-468. 2. Saxena, A. and Hudak, Jr., S. J., "Review and Extension of Compliance Information for Common Crack Growth Specimens," International Journal of Fracture, Vol. 14, No. 5, (1978) pp. 453-468. 3. Kapp, J. A., "Improved Wide Range Expressions for Displacements and Inverse Displacements for Standard Fracture Toughness Specimens," Journal of Testing and Evaluation, Vol. 19, No. 1, (1991) pp. 45-54.

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4. Simpson, L. A. and Clarke, C. F., "Application of the Potential-Drop Method to Measurements of Hydrogen-Induced Sub-Critical Crack Growth in Zirconium-2.5 wt% Niobium," Atomic Energy of Canada Limited, ARCL-5815 (1977). 5. Halliday, M. D. and Beevers, C. J., "The Measurement of Crack Length and Shape during Fracture and Fatigue," Beevers, C. J., Ed., Engineering Materials Advisory Services, Warley, U.K., (1980) pp. 85-112. 6. Schwalbe, K. H. and Setz, W., "The Measurement of Crack Length and Shape during Fracture and Fatigue," Beevers, C. J., Ed., Engineering Materials Advisory Services, Warley, U.K., (1980) pp. 267-271. 7. Hicks, M. A. and Pickard, A. C, "A Comparison of Theoretical and Experimental Methods of Calibrating the Electrical Potential Drop Technique for Crack Length Determination," International Journal of Fracture, Vol. 20, (1982) pp. 91 ~ 101. 8. Doig, P. and Abbott, K. R., "Single Specimen Fracture Toughness Testing of Low Strength Steel Plate Using the Direct Current Electrical Potential Method," Journal of Testing and Evaluation, Vol. 12, No. 5, (1984) pp. 297-304. 9. Bakker, A., "A DC Potential Drop Procedure for Crack Initiation and R-Curve Measurements During Ductile Fracture Tests," ASTM STP 856, (1985 ) pp. 394-410. 10. Frise, P. R. and Sahney, R., "Selection of a Potential Drop Crack Measurement System for Zirconium Alloy Specimens," Insight, Vol. 38, No. 2, (1996) pp. 96-101. 11. Jones, K. I. and Frise, P. R., "Temperature Effects on DC Potential Drop Measurements Made on a Zirconium Alloy Plate Specimen," Insight, Vol. 38, No. 5, (1996) pp. 341 -345. 12. Mills, W. J., James, L. A. and Williams, J. A., "A Technique for Measuring Load-Line Displacements of Compact Ductile Fracture Toughness Specimens at Elevated Temperatures," Journal of Testing and Evaluation, Vol. 5, No. 6, (1977) pp. 446-451. 13. Hellman, D., Rohwerder, G. and Schwalbe, K. H., "Development of a Test Setup for Measuring Deflection of Single Edge Notched Bend (SENB) Specimens," Journal of Testing and Evaluation, Vol. 12, No. 1, (1984) pp. 62-64. 14. "Standard Test Method for J-Integral Characterization of Fracture Toughness," ASTM E 1737-96. 15. "Standard Test Method for Measurement of Fatigue Crack Growth Rates," ASTM E 647- 95a.

- 146 - JAERI-Conf 99-009

DC Current Circuit

Fig. 1 Schematic diagram of the DCPD system

Fig. 2 Pull rod assembly for Hot cell testing

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2 Holes Dia.=4.25

\ 10.20 4.68 9.36 4.68 _L 10.20

8.50 3.00 17.00

21.25 5.00

26.26

Fig. 3 Configurations of curved compact tension specimen

'Y. ..v t ,s

.:>^ii: \

Fig. 4 Placements of current wires, voltage wires and LVDTs

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TCT

Fig. 5 Measurement of crack length on the specimen surface

1.4

Normalized by Vo at aoPto/W=0.50 Room Temperature 1.3 -

1.2 WV. =0.411+1.169

1.1 CANDU Room temperaturs 1.0 Unirradiation Test result -Linear fit 0.9 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80

Fig. 6 Potential drop as a function of crack length for curved compact tension specimen at room temperature. For 0.50

- 149 JAERI-Conf 99-009

Fig. 7 Fracture surface of a specimen tested at room temperature

800 -

600 _ © Secant © . Line © 3 o 400 • / e / © / m CANDU / © Room Temperature 200 ta • p Unirradiation' | © Test Result 0 f • I 1 . 1 i t i i 0.0 0.5 1.0 1.5 2.0 2.5 3.0 Aa (mm)

Fig. 8 J-R curve of curved compact tension specimen

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2.6 DEVELOPMENT OF A REMOTE CONTROLLED SMALL PUNCH TESTING MACHINE FOR NUCLEAR FUSION RESEARCH

Masao OHMI, Junichi SAITO, Toshimitu ISHII, Taiji HOSHIYA, Shiro JITSUKAWA0

Department of JMTR, Oarai Research Establishment, JAERI Oarai-machi, Higashi-Ibaraki-gun, Ibaraki-ken, Japan

1) Department of Materials Science and Engineering, Tokai Research Establishment

ABSTRACT

An accelerator-driven deuterium-lithium (d-Li) stripping reaction-type neutron source, such as the International Fusion Materials Irradiation Facility(IFMIF) planned by the International Energy Agency is recognized as one of the most promising facility to obtain test environments of high-energy neutrons for fusion reactor materials development. The limitation on the available irradiation volume of the irradiation facility requires the development of the small specimen test techniques (SSTT). Application of SSTT to evaluate the degradation of various components in the light water reactor for the life extension is expected to be also quite beneficial. A remote-controlled testing machine for the Small Punch (SP) and miniaturized tensile tests was developed at the hot laboratory of the Japan Materials Testing Reactor (JMTR). The machine is designed for testing at temperatures ranging between 93K and 1123 K to evaluate the temperature dependence of the strength of materials including the embrittlement at low temperatures and the softening at elevated temperatures in a vacuum or in an inert gas environment. The machine has been installed in a hot cell and is used for the round robin test program of the SP test method. The round robin test program was planned to identify the capability of the test method and to establish a standard test procedure. The configuration and the specifications of the test machine are introduced and the results of the round robin tests are also shown.

INTRODUCTION

For the plant life extension of commercial Light Water Reactors (LWR), the SSTT has begun to be applied to evaluate the performance of the on-site annealing of radiation hardened reactor vessels [1-3]. For the fusion reactor materials development, SSTT has been developed as one of the key technologies for an accelerator driven d-Li neutron source of which the irradiation volume will be quite limited [4,5]. Utilization of the small specimen also makes it

- 151 - JAERI-Conf 99-009 easier to control irradiation conditions, and reduces radio active waste. In the JMTR Hot Laboratory, a small punch testing apparatus has been developed and installed in a hot cell. The technical development of tests has been pursued in cooperation with JAERI Tokai since 1987.

Test Method, Apparatus and SP testing

1. Outline of SP Test A variety of punch test methods for transmission electron microscopy (TEM) disks have been developed. They are miniaturized to disk bend test (MDBT), SP test and shear punch test. The deformations of the specimen during the punch tests are complicated. This is especially true for MDBT and SP test. Empirical and analytical methods have been presented to extract tensile properties ( 6 y, 6 UTS, £ u and £ ,) from the load-displacement curves of the punch tests. The SP test is a method to deform a disk specimen, which is clamped by two jigs with holes at their center, by a spherically tipped penetrator (steel ball) (see Fig.l). A 3-mm- diameter TEM disk with a thickness of 0.25 mm and a rectangular plate of 10 mm square with 0.5-mm thickness are used as a specimen. Dimensions of the diameter of the steel ball, the lower holder hole diameter, and the radius at the shoulder of the lower holder for two types of specimens are also shown in Fig.l. Prior to the test, the holder is forced to clamp the specimen rigidly to limit specimen deformation in the region at the hole of the lower holder. Then the specimen is deformed at the center by punching with a steel ball. An example of the load-displacement curve of the SP test is shown in Fig.2 [6]. During the test, the deformation mode of the specimen changes successively; elastic bending, plastic bending, plastic membrane stretching, and plastic instability development stages. For hardened materials, which often exhibit smaller work hardening ability, the slope for plastic bending stage often increases and transition from the plastic bending stage to the plastic membrane stretching stage becomes invisible. It is indicated for the SP test that the load at the transition from the elastic bending stage to the plastic bending stage, the maximum load and the displacement at the maximum load

correspond to Oy , o UTS and £ u, respectively. The energy to fracture, which is obtained from a load displacement curve, may correspond to a toughness of the materials for the SP test. Efforts have been made by many researchers to obtain correlation between the toughness (SP energy) and fracture-related properties and between characteristics of the load- displacement curve and tensile stress-strain relationships. Baik et al.[6] demonstrated that the temperature dependence of the energy (elastic plus plastic energy) for some ferritic alloys showed a steep decrease with decreasing temperature in a narrow temperature range and that the transition temperature correlated well with a transition of the fracture mode; cleavage fracture had occurred at lower temperatures than the transition temperature. Suzuki et al. [7], McNaney et al. [8] and Misawa et al. [9] also showed that there was a simple relation between the transition temperature (SPDBTT) and the ductile brittle transition temperature (DBTT)

- 152 - JAERI-Conf 99-009 from Charpy V-notch (CVN) tests for several different steels. Takahashi et al. [10] and Suzuki et al. indicated that SP energy and the minimum thickness of the specimen at fracture also correlated well with the elastic plastic fracture toughness, JIC, of the materials obtained by ASTM standard test method for JIC measurement [11]. Okada et al. [12] and Suzuki et al. examined load displacement curves of irradiated and unirradiated alloys. Okada et al. pointed out that the maximum load of punch test correlated well with tensile strength, and Suzuki et al. reported that (tensile) yield stress exhibited a similar change with the transition load from the elastic to the plastic stage (see Fig. 2) by irradiation.

2. Testing Apparatus for SP Test In the JMTR Hot Laboratory, a test apparatus capable of SP testing and miniaturized tension testing has been developed and installed in a hot cell. As the machine is used in hot cell, care was taken to design it for easy manipulation of the specimen holder and operation of the machine. Fig.3 shows the schematic drawing of the remote controlled small punch testing machine. Fig.4 shows the inside of a vacuum chamber of the machine. To conduct tests, holders with specimen are placed first into the holes in the turntable by a manipulator. Then the turntable turns to a right angle, placing exactly one of the holders above a lower rod, and the lower rod travels upward to carry the holder to an upper rod. The lower rod thrusts the holder to the upper rod to apply force on the holder clamping the specimen between the upper and lower part of a holder. Finally, an actuator travels down to deform the specimen and the lower rod moves downward to place the holder on the turntable after the test. This sequence can be operated automatically by a computer until tests for 12 holders are finished. Fig. 5 shows a remote loading apparatus for the specimen holder. Another feature of this testing apparatus is in displacement measurement. Displacement during a SP test is usually obtained from the travel of the punch rod at the loading point. The actuator rod of this machine is relatively long and therefore can shrink elastically by compressive testing forces. Therefore, a displacement measurement rod equipped with a linear variable differential transformer (LVDT) is attached to the bottom surface of the specimen during the test to avoid disturbances by the deformation of the actuator rod. Table 1 shows current performance of the machine. The load is measured with an accuracy of 1%. The SP apparatus has an automatic specimen exchanger with a turntable that can test 12 specimens in a batch, under vacuum condition and at temperature ranging from 93K to 1123K. A test temperature is controlled with an accuracy of ±2K.

3. Performance Test of SP Testing In the JMTR Hot Laboratory, a final performance test of the SP testing apparatus before the round robin test was carried out in June 1995. A material used in the test was 2.25Cr-lMo steel with normalized and tempered heat treatment. The 2.25Cr-lMo steel is used for the pressure vessel of high temperature engineering test reactor (HTTR). Two types of specimens, 3mm in diameter and 0.25mm in thickness (TEM disk type) and those of 10 X 10 X 0.5mm (coupon type) were used for the test. The punching speed used was 0.5 mm/min.

- 153- JAERI-Conf 99-009

These tests were done in the temperature range from 113K to 248K. Results are in good agreement with those obtained by Suzuki, et al. Thus, it has been confirmed that the machine in the cell has good performance to obtain SP-related data. [13], [14]

4. Round robin Test A round robin test program for the standardization of SP test technique is under way. The Energy Materials Development Laboratory, JAERI-Tokai prepared SP specimens and distributed to the participants of this program. The participants are shown in Table 2 with types of specimens used for the test. [14] The procedures are shown in Fig. 6.

4.1 Materials and specimens Materials examined were a 2.25 Cr-lMo steel with three heat treatment conditions, NT (normalized and temperature), AN (annealed), and QT (quench and tempered). Specimens of 3mm in diameter and 0.25mm in thickness (TEM disk type) and those of 10 X 10 X 0.5mm (coupon type) were machined from a block of the steel. Table 2 indicates specimen types tested at each laboratory.

4.2 Results on the TEM disk -type specimens Load-displacement curves and SP energies of TEM disk type NT specimens are shown in Fig.7, 8, as functions of temperature. Though the trends were similar, there are some scatters SP energy results. The difference might be caused by; (1) The effect of specimen thickness (Oarai-NT-EP specimens are Electro-polished specimens of Oarai-NT specimens by 10% in thickness), (2) Methods of deflection measurement (elastic component of the displacement depends on the rigidity of the punch rod). In summary, although the largest difference in the energy is about 50%, the temperature dependence of SP energies by participants are similar, suggesting the test would be used estimating DBTT of the material.

4.3 Results on the coupon-type specimens The tendencies of the SP test data on coupon type specimens were similar to those for TEM disks, though the scatter of the data was smaller for the coupons. In Fig.9, 10, examples of the, load-displacement curves and SP energies of NT materials are shown as functions of temperature.

CONCLUSIONS

In the JMTR Hot Laboratory, the technical development for SP test has been pursued in cooperation with JAERI Tokai since 1987. Now, a small punch testing machine has been developed and installed in a hot cell. During the development, problems such as SP test machine development, test rig development, examination of specimen heating and cooling methods have been accomplished

- 154 JAERI-Conf 99-009

The SP test machine has an automatic exchanger with a turntable that can test 12 specimens in a batch under vacuum condition and in temperature ranging from 93 K to 1123K. A displacement measurement rod equipped with a linear variable differential transformer is attached to the bottom surface of the specimen during the test to avoid disturbances by the deformation of the actuator rod. In the future, dimension measurement device of specimen are expected to be developed. Results of this study are as follows; (l)No significant difference was observed between TEM disks and coupon specimens, though the latter gave rise to the less difficulties in the handling procedure and the smaller variation of area. (2)As to the SP energy obtained by research institutes in roundrobin test, the value of Oarai-SP energy was lower (about 5% ~10%) than the case of indirect measurement of cross head displacement by the testing equipment. (3)To obtain the absolute value for SP energy, the deflection should be measured directly from the deformation of specimen, e.g., using a linear variable differential transformer.

Acknowledgment

Authors would like to acknowledge to Dr Norikazu OOKA, deputy director of JMTR, for his helpful advice.

References [I] A. D. Amayev, et al.,ASTM STP 1204,1993,pp. 424 [2] M. Vallo and R. Ahlstrand, ibid., pp. 440-456 [3] A. T. Rosinski, et al., ibid., pp. 405 [4] G. E.Lucas, Metallurgical Transactions, 21 A, 1990, pp. 1105 [5] K. Noda, et al., J. of Nucl. Mater., 191-194 (1992) 1367 [6] J. M. Baik, et al., "Development of Small Punch Test for Ductile-Brittle Transition Temperature Measurement of Temper Embrittled Ni-Cr Steels", ASTM STP 888,1986, pp. 92-111. [7] M. Suzuki, et al., "Evaluation of toughness degradation by small punch (SP) tests for neutron-irradiated 21/4Cr-lMo steel", J. of Nucl. Mater., Vols. 179-181, 1991, pp. 441-444. [8] J. McNaney , et al., "Application of Ball Punch Tests to Evaluating Fracture Mode Transition in Ferritic Steels", J. of Nucl. Mater., Vols. 179-181, 1991, pp. 429-433. [9] T. Misawa, et al., "Determination of the Minimum Quantity of Irradiated Ferritic Steel Specimens for Small Punch DBTT Testing", J. of Nucl. Mater., Vols 179-181, 1991, pp. 421-424. [10] H. Takahashi, et al., "Standardization of SP test (in Japanese)", JAERI-M 88-172, JAERI, Ibaraki, Japan, 1988. [II] Standard Test Method for JIC, A Measure of Fracture Toughness, ASTM E 813-88, Vol. 03.01., ASTM, Philadelphia, 1988, pp. 698-712.

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[12] A. Okada, et al., "Microbulge Testing Applied to Neutron Irradiated Materials", J. of Nucl. Mater., Vols. 179-181, 1991, pp. 445-448. [13] S. Jitsukawa, et al., "Methods and Device for Small Specimen Testing at the Japan Atomic Energy Research Institute", ASTM STP 1024,, Philadelphia, 1993, pp. 289-307. [14] M. Ohmi, et al., "Development of Small Specimen Test Techniques ", J. at. Energy Soc. Japan, Vol.39, No. 11,1997, pp966~974. [15] M. Eto, et al., ASTM STP-1204,1993, pp241-255

Table 1 Specification of the SP testing machine Item Specification Test method Small Punch test Miniaturized tension test Load capacity 30kN Load cell 5kN (accuracy of 1%) Punch speed 0.003 ~3mm/min. Punch stroke 8mm Temperature range 93K~1123K(accuracyof ±2K) Vacuum rate 1.3X10-3Pa Clamping forces 0~5kN Displacement range 0.001 ~20mm Maximum number of holders 12 specimens in a batch in the vacuum chamber SP specimen 3mm-diameter and 0.25mm-thickness 10mmX10mmX 0.5mm-thickness Tension specimen 25.4mm-length and 1mm-thickness

Table 2 Materials,specimens and laboratories which participated in the round robin test. O : tested, -: not tested 2.25Cr-1Mo Steel Mate rials NT AN QT Specimens TEM Coupon TEM Coupon TEM Coupon Laboratories JAERI-Oarai o o o O o o JAERI-Tokai o o o o o o Hitachi — o — o — o Muroran — o — o — o PNL o — —• — — — NT:1173/1198K-5h,water-cooled,913/933K-6h,air-cooled,PWHT(950/963K-21 h) AN:1173/1203K-5h,cooled at 60K/h,PWHT(950/963K-21 h) QT:1173/1198K-5h,water-cooled,893/908K-4h,air-cooled,PWHT(868/883K-20h)

- 156 - JAERI-Conf 99-009

i;i Upi>«;i mi i.ii "" ol ball

I! '! 0 110mm 1 I I i

\, (•: • / Specimen 1 i • iiwer jig

Coupon type TEM disk type d1 0 2.4 01.0 d2 0 4.0 01.5 R 0.2 0.2 Steel Ball 56 2.4 01.0 Unitmm Fig.1 Cross sectional view of the specimen holder for SP test

disk type specimen Steel

ball. V •I f

0 Elastic bending stage ® Plastic membrane stretching stage

J ©Plastic bending stage ©Plastic iristability stage Py : Yield load Pmax.: Maximum load Pmax. Pf : Fracture load

m o Py,

Displacement (S)

Fig.2 Deformation mode during SP test

- 157 JAERI-Coni" 99-009

Load frame Ball screw ^Punching motor

Vacuum pomp Load cell

Bellows -Extensometer Punching rod Load cell Vacuum chamber Upper rod Specimen -LN2 evaporator holder -Window -Furnace

-Lower rod Turntable Motor-

Crosshead -Extensometer

Jo 20cm

Motor Fig.3 Schematic illustration of a remote controlled SP testing machine I

LN2 evaporator

Furnace

Air tweezers

Specimen holder Turntable

Fig.4 Photograph of the vacuum chamber of SP test machine

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Punch rod : stroke control

LN2 evaporator Furnace

Specimen holder

Turntable

10cm

T Lower rod : load control

Exchanging of the specimen holder J) Specimen holder loading Temperature control SP test Unloading of specimen holder 1 © Rotating of the turntable (by 30Xn degree)

Fig.5 Remote loading apparatus for the specimen holder

- 159- r SP Jest specimen ^ J •i6xi(>X0t'5i:t /3X0.25t J evaluation

tT n; ^rliQnfS ;SEM observatiV i"vJIOJJICtv

e qf=ln(to/t)

xfecfetermi nation 8 * 1 n o at fracture j o o SFenergy-dfspfecemervt pti o cqf=/3(S* /tO) determination Py and Pmax. (SPDBTT=(SPmax.+SPmin.)/2 c _ I Jic=k e qf-Jo k=345kJ/m2 $ y=362Py/tO2 c^uts = 130Pmax./t02-320

Fig.6 Diagram flow of PIE for SP test JAERI-Conf 99-009

0.6

0.5

110K 140K 0.4 180K 220K 298K

IS 0.3 o Z3 QL 0.2

0.1 2.25Cr-1Mosteel(NT), Non polishing ^3X0.25mmt Test speed 0.5mm/min Environment in vacuum

0 0.1 0.4 0.6 0.8 10 Displacement (mm) Fig.7 Load-displacement curves of TEM disk type NT specimens

0.45 Material: 2.25Cr-1Mosteel(NT) 0.40 V Specimen size: /3X0.25mmt w : Electro-polishing 8: Non polishing 0.35 o

0.30

0) 0.25 c n 0.20

0.05

0 100 150 200 250 300 350 Test temperature (K) Fig.8 SP energies of TEM disk type NT specimens (JAERI. M. Eto, et al.)

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110K 120K 140K 160K 180K 220K

0.4 0.8 1.2 1.6 2.0 Displacement (mm) Fig. 9 Load-displacement curves of coupon type NT specimens

3.0 Material: 2.25CM Mo steel(NT) Specimen size: 10X10X0.5mmt 2.5 D

2.0

E> 1.5 A Q) A © £L 10 • : JAERI Oarai.Hot lab. D : Muroran Univ. O : JAERI Tokai.Materials 0.5 Strength Lab. A : Hitati Lab. I I 100 150 200 250 300 350 Test temperature (K)

Fig. 10 SP energies of coupon type NT specimens (JAERI. M. Eto, et al.)

- 162 - JP9950637 JAERI-Conf 99-009

2.7 NEWLY DEVELOPED NON-DESTRUCTIVE TESTING METHOD FOR EVALUATION OF IRRADIATION BRITTLENESS OF STRUCTURAL MATERIALS USING ULTRASONIC

* Toshimitsu ISHII, Norikazu OOKA, Yoshiaki KATO, Junichi SAITO, Taiji HOSHIYA Saburo SHffiATA0 and Hideo KOBAYASHI2)

Department of JMTR, Oarai Research Establishment, JAERI Oarai-machi, Higashi-ibaraki-gun, Ibaraki-ken, 311 -1394 Japan

1) Ishikawajima-Harima Heavy Industries Co., Ltd. 2) Tokyo Institute of Technology

ABSTRACT Surveillance testing is important to evaluate neutron irradiation embrittlement of reactor pressure vessel material for long life operation. An alternative test method for evaluating the irradiation embrittlement of the pressure vessel material will have to be proposed to support the limited number of surveillance test specimens in order to manage the plant life to be extended. In this study, ultrasonic testing for irradiated A533B-1 steel and weld metal was applied to examine material degradation nondestructively. With increasing the shift of Charpy 41 J transition temperature, ultrasonic velocity decreased and attenuation coefficient of ultrasonic wave increased. Especially, the difference of ultrasonic velocity for 5 MHz shear wave between as-received and irradiated material is corresponding to the shift of transition temperature showing material degradation.

INTRODUCTION For the life extension of nuclear power plants, it is very important to detect aged deterioration of the materials used for structures and components such as a reactor pressure vessel (RPV). Since the RPV is exposed to neutron irradiation during the service period, the irradiation damage may occur to the RPV steel. Therefore, surveillance test to evaluate the irradiation embrittlement of the RPV material has been specified to the nuclear power plant. Irradiation capsules filled with the surveillance test specimens to measure the shift of Charpy transition temperature and the fracture toughness deterioration for the material of RPV are installed in the reactor [1]. As the number of those specimens will be insufficient if the plant life is extended, it is anticipated that the useful techniques of destructive or nondestructive test to support the surveillance testing is being required in the irradiation study. The reconstitution technique of Charpy impact specimens to be broken in the surveillance testing is indispensable for the implementation of destructive testing [2]. On the other hand, study on the nondestructive detection of the irradiation damage is also performed by measuring ultrasonic echo [3], positron annihilation [4], magnetic hysteresis [5] and neutron scattering [6] as a substitution for the surveillance testing. Nondestructive testing

- 163 - JAERI-Conf 99-009 technique for the irradiation embrittlement is very useful not only for the backup of surveillance testing but also for the reduction of radioactive waste which will be produced by surveillance testing. The main purpose of this study is to confirm the nondestructive evaluation method by using the ultrasonic wave for characterizing the irradiation embrittlement of the RPV material. As a first step, propagation time and echo amplitude of ultrasonic wave for the A533B-1 steel and weld metal, which were irradiated in the Japan Materials Testing Reactor (JMTR), were measured by remote manipulation in a hot cell of the JMTR Hot Laboratory. The irradiation damage of these materials is nondestructively evaluated on the basis of ultrasonic testing results.

EXPERIMENTAL PROCEDURE Three kinds of materials whose chemical compositions are shown in Table 1 were used in this study. The commercial A533B-1 (ASTM A533 gr. B cl. 1) steel is a material for the reactor pressure vessel. The Low P A533B-1 steel is melted in the laboratory to reduce the phosphorus content. The weld metal was fabricated by submerged arc welding. The configuration and dimensions of the Charpy impact specimen used in this study are in accordance with JIS Z2202. Test specimens were irradiated in the JMTR (thermal power: 50MW) at about 523 K or 563 K up to a fast neutron fluence of 1 x 1024 n/m2 (E>1 MeV). An annealing heat-treatment at 673 K for 5 min was applied to some of the irradiated specirnens in order to prepare the samples with the different embrittlement characteristics. The Charpy impact test of these specimens was performed in the lead cell of the JMTR Hot Laboratory, complying with the specification of ASTM A 370. Figure 1 shows the schematic diagram of the ultrasonic wave measurement system installed in the lead cell of the JMTR Hot Laboratory to examine the characteristics of the ultrasonic wave for the irradiated Charpy specimens. An ultrasonic probe fixed to the clamping rig was placed on the surface of the specimens by the manipulator to measure the propagation time and the pulse amplitude of the ultrasonic wave. A couplant to be used to propagate the ultrasonic wave from the probe to the specimen smoothly was both machine oil and glycerin. The size of transducer was 6.3 mm in diameter. The test frequencies of the ultrasonic wave are 5 MHz for share wave, and 10 and 15 MHz for longitudinal wave. Propagation time between first and second echo, and amplitude of these echoes were obtained from the pulse echo displayed on a CRT. After the ultrasonic testing, thickness of specimens was measured with accuracy of + 1 |Lim. The ultrasonic velocity and attenuation coefficient of materials were calculated by the following equations, respectively [7].

(Specimen's thickness) x 2 Ultrasonic velocity = (1) Propagation time between first and second echo

(Amplitude of first echo / Amplitude of second echo) Attenuation coefficient = — (2) (Specimen's thickness) x 2

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The longitudinal wave velocity, shear wave velocity and attenuation coefficient were obtained from the result of measurement.

RESULTS AND DISCUSSION Figure 2 shows Charpy impact test results and typical transition curves for the commercial A533B-1 steel irradiated at 563 K. Charpy transition curve for the as-received material was determined by fitting the data to the hyperbolic tangent equation [8]. The transition temperature at 41 Joule of absorbed energy for the as-received materials is 234 K. Assuming that the Charpy transition temperature for irradiated material is obtained by shifting typical curve for the as-received material to the irradiated material, due to the limited number of irradiated specimens. The shift of Charpy 41 J transition temperature (hereafter with transition temperature) for irradiated material will be estimated to be 225 K. The shift for the material annealed after the irradiation is to be 160 K in the same way. It is recognized that the embrittlement of the irradiated material is recovered by annealing at 673 K for 5 min. The transition temperature for the irradiated material may be estimated to be a smaller value against the real transition temperature to be measured because the maximum temperature of Charpy impact testing was also low. The data of transition temperature and its shift, which are estimated for three kinds of materials, are summarized in Table 2. Figure 3 shows the correlation between the ultrasonic velocity of 5 MHz shear wave and the shift of transition temperature for four kinds of materials. The ultrasonic velocity decreases with increasing the shift of transition temperature. It was found that the ultrasonic velocity of 5 MHz shear wave depends on the degree of embrittlement for the materials used in this study. The correlation between the ultrasonic velocity of 10 MHz and 15 MHz longitudinal wave and the shift of transition temperature is shown in Fig. 4 and Fig. 5, respectively. The velocity of both longitudinal wave decreases slightly with increasing the shift of transition temperature, but the scattering of data is observed in these figures. Figure 6 represents the difference of the ultrasonic velocity for 5 MHz shear wave between the as-received material and the irradiated material or annealed material after the irradiation. The value of the ultrasonic velocity difference decreases with increasing the shift of transition temperature. The good relation between the ultrasonic velocity difference and the transition temperature shift was obtained as shown in the solid line. Figure 7 shows the experimental data in case of 10 and 15 MHz longitudinal wave. The amount of velocity difference is smaller than that of the data for 5 MHz shear wave, and the scattering of data is observed. The solid and dotted lines showing the velocity difference for 10 and 15 MHz represent the good corresponding, respectively. Figure 8 shows the correlation between the attenuation coefficient of 15 MHz longitudinal wave and the shift of transition temperature. Attenuation coefficient increases with increasing the shift of transition temperature except for the data on the commercial A533B-1 steel irradiated at 523 K. Figure 9 represents the difference of the attenuation coefficient for 15 MHz longitudinal wave between as-received material and irradiated material or annealed material after the irradiation. The good relationship between the difference of the attenuation coefficient and the shift of transition

- 165 - JAERI-Conf 99-009 temperature was obtained as shown in the solid line. The sound pressure of ultrasonic in the irradiated materials becomes lower compared with the unirradiated materials, which may be related to the factor such as the helium void, vacancy and lattice defects induced by neutron irradiation [7,9]. It was found the NDE method by ultrasonic testing is applicable and indispensable for characterizing the irradiation embrittlement of material such as RPV or its component.

CONCLUSIONS The following relations between the ultrasonic characteristics and Charpy transition temperature for A533B-1 steel and weld metal were obtained. (1) Ultrasonic velocity decreased with increasing the shift amount of Charpy transition temperature. (2) The tendency that the attenuation coefficient of ultrasonic wave increased with increasing the shift of Charpy transition temperature was observed. (3) The difference of ultrasonic velocity for 5 MHz shear wave between as-received and irradiated material shows a good corresponding to the shift amount of Charpy transition temperature.

ACKNOWLEDGMENTS The authors would like to thank Mr. Yoneyama and Mr. Yoshida of Ishikawajima-Harima Heavy Industries co., ltd. for their technical supports. In addition, they are grateful to Mr. Baba and Mr. Onizawa for their helpful advice.

REFERENCES [1] Japanese Electric Association, "Fracture Toughness Test Methods for Nuclear Power Plant Components," JEAC 4206-1991. (in Japanese). [2] Y. Nishiyama, K. Fukaya, K. Onizawa, M. Suzuki, T. Nakamura, S. Kaihara, A. Sato and K. Yoshida, "Reconstitution of Charpy Impact Specimens by Surface Activated joining," Small Specimen Test Techniques, ASTM STP 1329, American Society for Testing and Materials, (1998), pp. 484-494. [3] H. Yoneyama, N. Ooka, Y. Futamura, T. Hirano, K. Yoshida and H. Kobayashi, "Study of characterizing irradiation embrittlement of pressure vessel steel by ultrasonic technique", PVP-Vol. 228, Nuclear Plant System/Components Aging Management and Life Extension, ASME(1992). [4] B. S. Viswanathan, D. Pachur, and R. V. Nandedkar, "Investigation of Neutron Irradiated Reactor Pressure Vessel Steel by Positron Annihilation and Electron Microscope," ASTM STP 956, (1987), pp. 369-379 [5] K. Ara, N. Ebine and N. Nakajima, "A New Method of Nondestructive Measurement for Assessment of Material Degradation of Aged Reactor Pressure Vessels," J. of Pressure Vessel Technology (Trans. ASME), Vol. 118, pp. 447-453, (1996). [6] I. E. Ukpong, A. D. Krawitz, D. F. R. Mildner, and H. P. Leightly, Jr., "A study of Radiation Induced Voids and Precipitation and Their Annealing Behavior by Small-Angle Neutron Scattering," ASTM STP 956, (1987), pp. 480-493.

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[7] Japan Society for the Promotion of Science (GAKUSHIN), "Ultrasonic Material Testing (Revised Edition)," The Nikkan Kogyo Shinbun, Ltd., Tokyo, (1984). (in Japanese) [8] K. Onizawa and M. Suzuki, "Correlation among the Change in Mechanical Properties due to Neutron Irradiation for Pressure Vessel Steel," ISIJ International, Vol. 37 (1997), No. 8, pp. 821-828. [9] S. Ishino, "Irradiation damage", Tokyo University press, (1979). (in Japanese)

Table 1 -- Chemical composition. [Wt%] C Si Mn P S Ni Cr Mo Cu Commercial A533B-1 steel 0.22 0.31 1.36 0.01 0.012 0.58 0.13 0.52 0.14 Low phospholus A533B-1 melted in Labratory 0.21 0.28 1.36 0.003 0.01 0.6 0.11 0.51 0.16 Weld metal 0.076 0.23 1.46 0.016 0.01 0.66 0.037 0.47 0.089

Table 2 — Charpy transition temperature (and its shift). [K] As recieved Irrad.+Annealed Irradiated Commercial A533B-1 steel irrad. at 523K 234 439 (205) 484 (250) Commercial A533B-1 steel irrad. at 563K 234 394(160) 459 (225) Low P A533B-1 steel irrad. at 563K 199 303(104) 403 (204) Weld Metal irrad. at 563K 217 357(140) 477(260)

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Operatioionn) Manipulator area J Data processing i Hot cell unit Ultrasonic test instrument Clamping rig of probe \5

Probe-—i

Irradiated j charpy - impact specimen'

Fig. 1 — Schematic view of experimental apparatus for nondestructive evaluation of iiTadiation embrittlement in hot cell.

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5 50"- i° O X o 0 100 200 i 30i 0 400 500 600 Test temperature (K) Fig. 2 — Charpy impact test results for commercial A533B-1 steel.

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Fig. 3 -- Correlation between ultrasonic velocity of 5 MHz shear wave and shift of Charpy transition temperature.

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0 50 100 150 200 250 300 Shift of Charpy transition temperature (K) Fig. 8 — Correlation between attenuation coefficient of 15 MHz longitudinal wave and shift of Charpy transition temperature.

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2.8 Reassembling Technique for Irradiation vehicle at Fuel Monitoring Facility (FMF)

Koji MAEDA, Tsuyoshi NAGAMINE, Yasuo NAKAMURA, Takeshi MITSUGI and Shinichiro MATSUMOTO

O-arai Engineering Center, Japan Nuclear Cycle Development Institute (JNC) 4002 Narita-cho, O-arai machi, Higashi ibaraki-gun, Ibaraki-ken, Japan

ABSTRACT

The remote handling technique has been developed and demonstrated by Fuel Monitoring Facility (FMF) operated by Japan Nuclear Cycle Development Institute (JNC). In particular, the reassembling of irradiated fuels has been successfully performed, and reassembled irradiation vehicles were reinserted to Japanese experimental fast reactor "JOYO".

1. INTRODUCTION The Fuel Monitoring Facility (FMF) is located adjacent to the experimental fast reactor "JOYO", at Oarai Engineering Center of Japan Nuclear Cycle Development Institute. At FMF, approximately 200 assemblies have already been disassembled and examined, and obtained results have been fed to the analysis and evaluation of fuel performance. In addition to these once-through examinations, the interim examinations and the reinsertion for continuous irradiation have been conducted to develop high bumup fuel and/or high neutron dose material. The continuous irradiation gives more flexibility for the irradiation experiments. Since the FMF was originally designed to make the reinsertion possible, there is a path to send the. assembly back to the reactor. The main items developed for the reinsertion of assemblies were as follows; (l)Irradiation vehicle, (2)Disassembling and interim examination, (3)Decontamination of fuel pin or structural materials encapsulated, (4)Reassembling machine. Figure 1 shows the materials flow of the reinsertion. After the irradiation in "JOYO", the irradiation vehicle is transferred to the examination cell of FMF by the underground cask car without removing the remained sodium. In the examination cell, the sodium removal, disassembling the irradiation vehicle and the interim examinations of fuel pins or encapsulated structural materials are conducted. Then, fuel pins or capsules are transferred to the decontamination cell and decontaminated their surface. After the decontamination, they are transferred to the clean cell and reassembled into the irradiation vehicle respectively. The irradiation vehicle is sent back to the reactor by the cask car again. This paper describes following four items; (A)Irradiation vehicle, (B)Disassembling and interim examination, (C)Decontamination of fuel pin or capsule, (D)Reassembling machine, which are necessary for the reinsertion.

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2. IRRADIATION VEHICLE For the reassembling and reinsertion, it was necessary to develop the irradiation vehicle which was easy to disassemble and reassemble by remote handling without giving any damage to the fuel pin or the specimen capsule. The irradiation vehicle was developed and the modification in the structure of the vehicle was conducted through the mock-up test of disassembling and reassembling. Figure 2 shows the structure of the irradiation vehicle. It has same outside configuration as "JOYO" driver fuel assembly. That is; the vehicle is hexagonally shaped, 81.2mm across the outside pad faces and 2,970mm long. At above and below the pads, the face to face distance is 78.5mm. The vehicle contains 6 compartment tubes. Each compartment tube is fixed to the vehicle by being attached to the handling head and locked with the locking-nut. In each compartment tube, 5 fuel pins are tied to the tie rod and a temperature monitor block is also attached to a tie rod Thus the vehicle has the capability to irradiate 30 fuel pins simultaneously. Either wire-spaced or grid-spaced fuel pin can be loaded into each tube. Either fuel pin is 1,750mm long and outer diameter is 6.5mm. And wire-spaced fuel pin is wrapped with the wire on 172mm pitch. In addition, materials irradiation vehicles were developed to obtain irradiation data on various structural materials; core and absorber materials. These vehicles have also same outside configuration as "JOYO" driver fuel assembly and contain 6 compartment tubes. Instead of fuel pins, any mini-size specimen or absorber materials encapsulated are installed in compartment tubes respectively. Simultaneously, various fuel pin or structural materials can be installed in a same irradiation vehicle respectively. In addition, the coolant flow rate in each compartment can be controlled separately. Therefore systematic irradiation test can be conducted by the irradiation vehicle.

3. DISASSEMBLING AND INTERIM EXAMINATIONS The disassembling is conducted in the examination cell of FMF after the sodium removal. The interim examinations of fuel pins or capsules are also conducted in the examination cell. In case of fuel pins, main test items are weighing, visual inspection, laser profilometry and j -scanning. The purpose of these interim examinations are to confirm that fuel pins or capsules are intact and that the criteria for the reinsertion is satisfied. In case of structural materials encapsulated, capsules are transferred to the Materials Monitoring Facility(MMF) at the Oarai Engineering Center by a container And detail interim examinations and reassembling of capsules are conducted there. Therefore, interim examinations of fuel pins are mainly described here.

3.1 DISASSEMBLING Disassembling is conducted with the use of existing disassembling machine. The irradiation vehicle was designed to be disassembled without duct sectioning. The disassembling is conducted by unscrewing the locking-nut inside the handling head with a tool. The master slave manipulators are used to take off the handling head by rotating the handle of the tool. After that, the compartment tubes are pulled out from the duct. The compartment tube is disassembled by unscrewing the cap(Figure 3). And the fuel pin bundle or capsules are pulled out from the compartment tube. After that, each fuel pin is taken off from the tie rod(Figure 3). Capsules are also pulled out from the compartment tube.

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Disassembling processes are performed without any trouble. In addition, this procedure made possible to disassemble without giving any damage on fuel pins or specimens.

3.2 INTERIM EXAMINATIONS A. LASER PROFILOMETRY Pin profilometry is important technique for evaluating the irradiation performance of fuel pins. In case of reinsertion program, the removal of the wrapping wire is not acceptable, because it is required that the disassembled fuel pins are reassembled after interim examination as they were Therefore non contact type measuring system is important to be developed in order not to remove the wrapping wire. Laser system was introduced instead of conventional contact type measuring system. Figure 4 shows the schematic diagram of the pin profilometry system. The profilometry system consists of the scanning device in the examination cell and the control system in the operation area. He-Ne gas laser(6,330 A-wave length, lmW-power) system is used for the measuring device and it is surrounded by 5cm thick lead block as radiation shielding material. Owing to this shielding material, the life of this apparatus becomes 30 times longer than it was. The disassembled fuel pins are measured with the laser profilometry system as shown in Figure 5. The example of axial distribution of pin diameter measured by this system are shown in Figure 6. In this examination, length and diameter changes in the fuel pins, the changes of the wrapping wire pitch and fuel pin bowing are investigated. Accuracy in measurement are less than ± 0.5mm for length, less than ±3 ym for diameter and less than ± 0.5mm for the bowing.

B. r -SCANNING 7 -scanning is a non-destructive technique for determining the distribution of radioactive nuclides, such as fission products and activated fuel. A spent fuel emits 7 -ray and it gives a lot of information on the irradiated behavior of the fuel in a reactor. In addition to the technique for determining the axial distribution of radioactive nuclides, the computer tomography technique of a fuel pin were developed at FMF. It can be used as a reference information, especially in case of the interim examination of irradiated fuel pins for reinsertion. The programing and calculating technique used here, is based on a technique developed at Los Alamos National Laboratory, called MART (multiplicative algebraic reconstruction technique). The program for the emission tomography was developed by several improvement of MART.

Figure 7 shows the schematic diagram of the 7 -scanning system. The 7 -scanning system used in the measurements for a fuel pin consists of four components; (a) a scanning mechanism for the precise positioning of an irradiated fuel pin, (b) a collimator for the precise definition of the volume segment from which the 7 -ray spectra are collected, (c) a high-resolution detector assembly, (d) an automated data acquisition unit. The individual movement; X, Y, Z, are positioned with a precision of 0.01mm and the motion of rotation is set with a precision of 0.01 ° . Collimation of the 7-ray beam is required to obtain the necessary 7 -ray intensity per unit area. The width of collimator slit can be enlarged up to 1.2mm continuously. The detector assembly consists of Ge detector that the resolution is 2.0keV (FWHM) and MCA (multi channel analyzer) with 4096 channels. The data acquisition unit is automatically operated to

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control the scanning mechanisms as well as to collect and analyze 7 -ray spectra. Three types of investigation were performed to the fuel pins; (a) the determination of the axial distribution of radioactive nuclides, (b) the computer tomography, (c) the detection of Xe-133 at the pin plenum. There are some falls correspond to pellet gaps in the axial distribution profile of radioactive nuclides. From the diametral scan and the projection at six angular orientations, 7 -ray emission tomographs are obtained Figure 8 shows the reconstruction of Zr-95 and Cs-137. The existence of small central hole in the fuel pellet is observed from the distribution of non-volatile nuclides, Zr-95. And the volatile Cs migration into the pellet-cladding gap is observed by the distribution of Cs-137. Instead of puncturing test, the spectrum of Xe-133 is measured at the plenum in the fuel pins. Detection of Xe-133 at the plenum part confirms no leakage from the fuel pins.

C. OTHER EXAMINATIONS Visual inspection, X-ray radiography and weighing were performed to the fuel pins in addition to laser profilometry and 7 -scanning. The integrity of the fuel pins are confirmed by means of non-destructive examinations. In addition, destructive examination is usually performed to one fuel pin. All the results are strictly examined in comparison with the criteria for the reinsertion of fuel pins.

4. DECONTAMINATION of FUEL PIN SURFACE Before sending pins to a work station where the reassembling machine is located, the surface of all fuel pins should be decontaminated Because the examination cell has been contaminated by radioactive materials produced from sectioning of fuel pins. When the decontamination of fuel pin surface was conducted, it is required not to give any damage on fuel pin surface and a wrapping wire. The decontamination is performed with the use of felt ring. The process of the decontamination is as shown in Figure 9. All fuel pins are decontaminated at the level of less than 50,000dpm/pin (a contamination) in order to satisfy the criteria of the decontamination.

5. REASSEMBLING MACHINE It is required for the reinsertion to the fuel pins without any damage. The reassembling machine (Figure 10) was developed and installed in clean cell. Since destructive examination is usually performed to one fuel pin, the 29 disassembled fuel pins and one fresh pin are reassembled into a new irradiation vehicle. The bundle which consists of 5 fuel pins attached to a tie rod, is inserted to a compartment tube as shown in Figure 11. Then the compartment tube is capped After capping 6 compartment tubes, they are inserted to the duct as shown in Figure 12. Then a handling head is attached at the top of the duct and a locking-nut is screwed There is a pin by which the locking-nut won't rotate during the irradiation. The reassembling is finished after the confirmation that the pin is pushed up as shown in Figure 13. Up to now, 4 vehicles were successfully reassembled and 83 test fuel pins were reloaded to the reactor "JOYO". Though current regulation limits of irradiation for JOYO driver fuel pin is 75GWd/t, owing to the continuous irradiation, the achieved burnup and neutron dose are approximately 120GWd/t and 1.7X 1027 n/m2 (E>0.1MeV), respectively. In addition, 5 structural material vehicles were also successfully reloaded.

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6. FUTURE DIRECTIONS Reassembling technique for continuous irradiation will give more flexibility for the specific irradiation experiments and contribute to obtain various information on irradiated fuel behavior at high bumup an^or high neutron dose level. Besides the existing irradiation vehicles, advanced irradiation vehicles are being developed to enable irradiation tests in specific condition; precise irradiation temperature control, run to cladding breach, etc. Consequently, some minor modification will be made through the mockup testing of the equipments in order to handle those new type vehicles too. In addition, the FMF has introduced X-ray computer tomography into its extension building. X-ray CT test will give the tomograms and scanograms of assembly and fuel pins. Thereby, it is able to inspect inner state of assembly and fuel pins, non-destructively. Those test equipments will be put into hot operation soon and produce various information on irradiated fuel behavior.

7. CONCLUSION The FMF has demonstrated its capability in the remote handling technique for reassembling of irradiation vehicles. The reassembling technique for continuous irradiation test has contributed to increase achieved bumup and/or neutron dose. Up to now, 4 vehicles were successfully reassembled and 83 test fuel pins were reloades to the reactor "JOYO". The achieved burnup and neutron dose are approximately 120GWd/t and 1.7 X1027 n/cm2 (E>0.1MeV), respectively. In addition, 5 structural material vehicles were also successfully reloaded. The FMF has introduced X-ray computer tomography into its extension building. The X-ray CT tomograms and scanograms of assembly and fuel pins are especially expected to inspect inner state of assembly and fuel pins, non-destructively.

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Transfer cart of the cask Service Area

Examination Decontamination \-

o JOYO Cask Car o I Pin Visual Pin Reassembling Prohlometry Examination ^-scanning

FMF Cask Car

.' Receipt i .* Shipment I Cask Corridor

Figure 1 Materials Flow of Reinsertion JAERI-Conf 99-009

Handling Head- Lock ing-nut -

Duct. Fuel Pin

Outer Tube of Middle Pad- Compartment Inner Tube of Compartment 2970mm ie Rod Central Tube

Duct Cross Section

Entrance Nozzle o a

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Figure 3 Disassembling of Compartment Tube

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In Cell Cell Wall Operation Area

Figure 4 Schematic Diagram of Pin Profilometry System

Figure 5 Laser Pin Profilometry

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Figure 6 Axial Distribution of Pin Diameter JAERI-Conf 99-009

Scanning Mechanism Scanning Control Mini-Computer Syslem tollimator 1Fuel Pin y-ray Detector Computer

Multi-Channel Analyzer

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Figure 7 Schematic Diagram of j -scanning System

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Figure 8 y "rav Emission Tomographs of Radioactive

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Fuel Pin. Felt Ring

Container Tool for Felt Ring Fixture Felt ring insertion.

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Figure 11 Bundle Insertion

Figure 12 Inserted Compartment Tubes

- 186 > fd 2 n 00 o 3

Figure 13 Pin Pushing-up JP9950639

2.9 The Development of Electric Discharge Machine for Hot Cell Usages

Wanho OH*, Sangbok AHN*, Sangchul KWON**, Yongsuk KIM** , Keysoon LEE* Korea Atomic Energy Research Institute P. O. Box-105, Yusong, Daejon, Korea

ABSTRACT

The electric discharge machine (EDM) has been developed to fabricate the test specimens directly from the irradiated CANDU pressure tubes in hot cell. The machine was composed of mainly two parts, which were main body to discharge cutting specimens including filter unit and electric and control part. The whole layout size of main body is 1000(W)x905(D)x800rnm(H). The maximum size of plate work piece was 300(X)x200(Y)xl00mm(H) and specially chucking device could fully rotate for tube type material. The work tank sizes is 450(L)x 350(W)x250mm(H) and the volume of discharging oil were 80 liters. The electrode was attached to the head in the method of air chuck with 6- bar compressed air. The discharge conditions were set by computer numerical controls. The tests with various operation conditions were performed to get the optimum conditions for fabricating specimen from Zr-2.5Nb tube materials. The heat affected zone size from hardness test was about lOOfim in depth from cutting edges. The average and maximum roughness were 5~7|J,m and 30~60u;m with various input current conditions. The maximum specimen temperature was reached up about 90°C acquired from embedded thermocouple test. The specimen shape deformation acquired from discharge cutting was about IOOUJTL in the edge surface. The detailed specifications and the effects of specimen from discharge conditions were discussed.

* Irradiated Material Experimental Facility

** Zirconium Development Team

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INTRODUCTION

The fabrication test specimens in hot cell from irradiated work pieces is difficult and high techniques. Furthermore it is almost impossible to fabricate from parent materials with retaining original shapes by ordinary methods. Therefore many workers in irradiated material test parts have adopted the EDM for it with his own techniques. The hot cell equipments should be developed with compact dimension and easily maintenance. Furthermore the radiation degradation of parts should be considered. For the test of irradiated CANDU pressure tube in hot cell KAERI had developed the EDM for hot cell usages with these requirements.

SPECIFICATION

The machine was mainly composed of two parts. One is main body installed in hot cell as Photo 1, the other is electric and control part installed in operating area as Photo 2. The utility lines were electric, control line, control line and so on. The electrode height of the machine on working table in hot cell was coincided with the eye-sights of workers in operating area. The sizes were changed comparing to regular products, lower in height and larger in width. The sizes of main body were 1000mm(W)x905mm(D)x800mm(H). The detailed specifications are as follows

1. Main body The main body are composed of bed, head, work table and working oil filtering system. The layout is shown in Figure 1. l)Bed The bed supports the column, saddle and work tank. The total weight of main body was about 900kg. It has 4-leveling block to adjust the height and level of whole machine 2) Head

- 189 - JAERI-Conf 99-009

The head has the function of attachment electrode to the machine and discharge cutting of the parent materials. It is composed of body, sliding ram and air chuck. It can be moved to X, Y, Z-direction according to inputted signal from control computer. The coverage of electrode to cut specimen is 450(L)x350(D)x250mm(H), which means the maximum working sizes. The sliding ram moves with the combination of ball screw and linear bearing motion transferred from servomotor revolutions. In the ram system, the cross roller bearings are installed at the part of rolling motion area to promote the movement precisely. Additionally it can be operated without providing lubricants for long operation time. To attach the electrode easily with manipulator the special air chuck system adopted. It is operated with 6 bar compressed air. 3) Working table The working table is for fixing the work pieces to be cut. It is designed to fix tube and plate type pieces. It is also possible to fix another type materials when auxiliary plate is changed. The chuck to fix tube has the function of fully rotating refer to C-axis. The box for working table moves up with working oil during cutting works. Figure 2 shows the detailed table layouts. 4) Working oil supply and purification system It has the function of supply oil to work tank and filtering the impurity, which was produced during discharging. It was installed at the next of main body in hot cell. It has the oil pump and filtering unit. The unit was designed to exchange filter easily in hot cell with manupulators and 100 liters per minute in capacity. 5) Electrode The material for electrode was 3% Cr-Cu to protect excessive consuming from cutting heat. In the case of Zr-2.5Nb work piece materials electrode was larger or smaller than specimen in required sizes. The consuming tolerance was about lOO^im. The electrode is shown in Figure 3.

2. Electric and control system The main power of input electric is 3Ph-440V for machine. It transformed to appropriate

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demanded voltages for each parts. The flow chart of electric and control parts are shown in Figure 3. The main computer has the function which is control and transfer the operating signals to the main body through the RS-232C port. The control signal can be inputted from panel or portable key board. Photo 4 shows the monitor view in operating. In computer the APOS main board are adopted to convert the commands to electric control signals. It seperates signals to position control and operating signals and tranferred to pulse and sub CPU board individually. The APOS sub board generates the differential analog signal which comes from position control and encorder signals. They are sent to the servo amplifier. The position control signals from APOS sub board make the servo-motor rotated with variable speed. The encorder attached to motor detects the amount of rotation and it transferred to the APOS sub board. The operating conditions inputted from key board are changed to the signals at pulse generator(PG). The PG produce on-off time signals through MOS-FET. The signals are sent to the servo-motor and electric power controller. Another function of PG is the detection of abnormal discharge from feeding back signals. The rectifier makes the alternating current to direct current and maintains the uniform voltage conditions.

PEFORMANCE TEST

The following characterization tests were performed in order to check the effect to cutted material from discharge processing. The optimum cutting condition were decided for Zr- 2.5Nb tube materials.

1. Dimensional change In the process of discharging, the work piece material is consumed with discharging spark. This should be considered to make the electrode to fabricate precise specimen in dimension. For this the dimension inspection were performed using rod electrode which had 5mm in

- 191- JAERI-Conf 99-009 diameter. The hole diameters of work piece after discharging were 5.16-5.22mm in diameter with 4-15 amperes conditions.

2. Surface roughness The surface roughness created by the electric discharge machining process is of special interest because it has been shown to have a negative effect on the mechanical properties. The surface roughness with various conditions was measured. The cutting conditions were 4-15 Amperes in currents and 2fisec on time in discharging intervals. The average roughness was mainly increased with currents. The maximum roughness was rapidly changed from 30 to 60fim with increasing currents. The test results shown in figure 4.

3. Heat affected layer In the course of discharging the cut material was thermally affected with heats from electrical sparks. The heats make the materials a kind of thermal quenching. It makes specimen surface hardened and may change the mechanical and metallurgical properties of the surface.[l] [2] Therefore the micro-hardness, Hv test were performed in depth from discharged surface and the results are in Photo 5 and Figure 5. The cutting condition was 7 amperes in currents and 2|isec on, 5|isec off in discharging time intervals. From the figure the hardness decrease rapidly with the depth from surface in 0~100fXm ranges. It becomes original value of raw material far about lOOfim from the surface. This means that the heat affected depth is the range to about 100|im.

4. Heat-up temperature In the process of discharging the electrical energy would be transformed to thermal heat with sparking between work piece and electrode. The heat raises the temperature of whole specimen body and may give the sensitive effects in metallurgy, surface conditions and so on. To measure the temperature changes of cutting area in discharging the thermocouple was attached as Figure 6. The temperatures were monitored and recorded in the course of discharging. Figure 7 shows the temperature changes in specimen with time. The temperature

- 192 - JAERI-Conf 99-009 was rapidly raised at the beginning stage of discharge and it went the maximum temperature smoothly at the end. In the case of CANDU tubes the maximum temperature was about 80~90°C. This temperature would not effect the mechanical properties because of under the recrystallization temperature.

CONCLUSION

KAERI has developed EDM for hot cell usage. It will be used to fabricate test specimen from irradiated work pieces. For cutting specimen from irradiated CANDU tube, various tests were performed with cutting conditions. The results were the maximum 30~60|im in surface roughness, ~100|im in heat affected layer and 80-90 °C in specimen heat up temperature. The optimum condition to cut the CANDU tube were decided 7A in current and 2p.sec in on-time. For one specimen it is consumed normally 3-3.5 hours.

REFERENCE

1. John E. Fuller, The EDM surface: Topography, Chemistry, and Metallurgy, RFP-4498, 1991 2. John E. Fuller, Metallurgical effects from conventional EDM, and electrochemical drilling, RFP-3066, 1990

- 193 - JAERl-Conf 99-009

•.. \

il --'"i:;

Photo 1. The EDM view of main body in hot cell

f J '••;". i 1

I - • ..' i •.-

Photo 2. The electric control part of EDM in operating area

194 - JAERI-Conf 99-009

Figure 1. The layout of main body

Figure 2. The layout of the working table box

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3 «

Photo 3. The various electrode for EDM

Panel Key Bo Portable Key B N U RS-232C Port Transformer 440V to 110 Main Computer APOS Main APOS S

Magnet Controll t Pulse Controller Encoder

Resistance Part Servo Motor Transformer 440V to 70 AC-DC Rectifie Work Piece Transformer 440V to 85, 15 Servo Amplifier -4-

Figure 3. The flow chart of electric and control system for EDM

- 196 JAERI-Conf 99-009

Photo 4. The computer monitor in operating

60

© 40

o • Rmax Cum] D 0> Ra Cum] o 20

3 to

2.5 5.0 7.5 10.0 12.5 15.0 Input Current [A]

Figure 4. The maximum and average roughness of discharged surface

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200

Depth from Discharged Surface [|im]

Fiure 5. The hardness variation with depth from discharged surface

Electrode w i. 4mm x 40mm (Inner) t= 1.5mm

Work Piece Embedded Thermocouple t = 4.2mm Depth = 1 mm

Fiure 6. The apparatus of embedded thermocople in cutting specimen

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100

3.0 0.S 1.0 1.5 2.0 2.S 3.0 Discharging Time [h]

Figure 7. Temperature variation with discharging time

Photo 5. The indentation marks of micro hardness test surface

- 199 - JAERI-Conf 99-009 JP9950640

2.10 Development of Remote Laser Welding Technology

Soo Sung KIM, Woong Ki KIM, Jung Won LEE, Myung Seung YANG, Hyun Soo PARK

Korea Atomic Energy Research Institute P.O. Box 105, Yusong, Taejon 305-600, Korea Tel:42-868-8844, Fax:42-868-8824, E-mail:[email protected]

ABSTRACT Various welding processes are now available for end cap closure of nuclear fuel element such as TIG(Tungsten Inert Gas) welding, magnetic resistance welding and laser welding. Even though the resistance and TIG welding processs are widely used for manufacturing of the commercial fuel elements, it can not be recommended for the remote seal welding of fuel element at PIE facility due to its complexity of the electrode alignment, difficulty in the replacement of parts in the remote manner and its large heat input for thin sheath. Therefore, Nd:YAG laser system using the optical fiber transmission was selected for Zircaloy-4 end cap welding. Remote laser welding apparatus is developed using a pulsed Nd:YAG laser of 500 watt average power with optical fiber transmission. The laser weldability is satisfactory in respect of the microstructures and mechanical properties comparing with the TIG and resistance welding. The optimum operation processes of laser welding and the optical fiber transmission system for hot cell operation in remote manner have been developed.

INTRODUCTION Various studies have actively been conducted for developing a new nuclear fuel and manufacturing a capsule for its irradiation test. In such studies, a remotely controlled welding work have been required to be performed in a highly radioactive hot cell for manufacturing the nuclear fuel. [1,2] Meanwhile, the laser has been considered for the remotely controlled welding work since the optical fiber transmission system is easy for the laser welding in the shielded facility, but there is also a technical challenge of securing higher welding quality in the laser welding work. According to the process of manufacturing the nuclear fuel, the end cap welding of the fuel element is to weld Zircaloy-4 cladding tube which is charged with pellets with the end cap. Such end cap welding requires high reliability since if there is a defect in only one single point on the circumference of the fuel element welding, it will cause

- 200 - JAERI-Conf 99-009 the radioactive fission products to leak therefrom during combustion of the nuclear fuel, and consequently bring about a serious safety problem. [3] This study was conducted to develop optimum conditions for the laser welding system and to evaluate the performance of the weld zone in sealing the Zircaloy-4 end cap of the PHWR nuclear fuel element.

Development of Laser Welding Device & Optical Fiber Transmission System

1. Schedule of Development The schedule of development is shown in Table 1. There are two phases in development period, of which the first phase is to fabricate welding devices, and its installation and cold test from 1998. The second phase is to conduct the end cap welding of the nuclear fuel element utilizing spent nuclear fuel in the hot cell from the second half of 1999.

2. Laser Welding Equipment The remotely controlled welding chamber was manufactured as shown in Fig. 1 utilizing Nd:YAG laser system with optical fiber transmission system in order to welding of the end cap of the nuclear fuel element in hot cell. The welding chamber comprises of a body, a rotary driving section, an end cap inserting section, an optical fiber and a coupler section. When the beam oscillating from the laser system is transmitted, the optical fiber which is very flexible is utilized for the transmission. Since the distance between the welding stage in the hot cell and the laser system outside the hot cell was about 20M, an optical coupler was required for connecting the welding chamber with the optical fiber, As illustrated in Fig. 2, the optical coupler was manufactured in such a way that it enable the optical fiber, the optical fiber connector and the coupler to be replaced easily. 3. Fiber Transmission System In case the beam oscillating from Nd:YAG laser system is directly casted, its degree of positional freedom becomes poor and it is inconvenient to use the beam in a narrow space. Therefore, the optical fiber, which is very flexible, thin and long, is used. The optical fiber transmission system comprises of an optical inlet coupler, an optical fiber and an optical outlet coupler. The optical inlet coupler is a section where the beam is connected with an internal part of the core of the optical fiber by an incident lens. The optical fiber, which is

quartz glass of pure SiO2, comprises of a core part having a wide refractive index and a cladding part having a narrow refractive index, where diameters of the core are 600, 800 and 1000 jM, respectively, This is SI (Step Index) multi-mode type, and its NA (Numerical

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Aperture) of the optical fiber is 0.22. The focusing lens of the coupler used is UV grade fused silica.

RESULT AND DISCUSSION

1. Test of Remotely Controlled Laser Welding 1.1 Evaluation of Welding Performance The geometric joint configuration has a significant effect on the end cap welding. Any improvement in the geometry of the welding joint is of advantage to the autogenous process. If coagulation is brought about only in one direction while welding, it can be easy to melt it. Usually, laser welding causes a molten pool in the material more easily than TIG welding, and a deep weld penetration can be made by laser welding. Fig. 3 shows typical sectional view of TIG welding and laser welding in the end cap welding of the Zircaloy-4 cladding tube. As shown in Fig. 3, laser welding was found to have HAZ(Heat Affected Zone) much smaller comparing with TIG welding. Moreover, TIG welding usually had the larger melting volume comparing with laser welding, which melt by the focusing energy.

1.2 Characteristics of Laser Beam Transmission by Fiber Connector Considering the high radioactivity in the hot cell, the optical fiber connector was developed to be installed in the upper part of the welding chamber so that any contaminated optical fiber could be immediately replaced with new one by the remote control. Moreover, the optical fiber from the optical inlet coupler outside the hot cell to the optical fiber connector inside the hot cell is can be replaced when it is contaminated. In this study, the optical fiber of dia. 600 fM was used from the laser head to the optical fiber connector, and then the optical fiber of dia. 800 pm or another optical fiber of dia. 1000 im was used from the optical fiber connector to the optical outlet coupler because the beam focused on the collimatng lens had to be within the largest allowable range in consideration of the characteristics of the law of the beam quality preservation. The welding experiment was conducted under the following conditions of the optical outlet coupler representing the optical fiber of dia. 800 pm, F#=2, focal length of the condenser (FL) = 95 mm or 120 mm, the optical factor = 1.35 or 2.1. In case the optical factor is 1.35, the weld penetration was found to be greater at FL = 95 mm than at FL = 120 mm. In case the optical factor is 2.1, the bead was found to be 1.8 mm at FL = 120 mm, which was wider than that of FL = 95 mm by 0.3 ~ 0.4 mm. In case FL is 95 mm and the optical fiber of dia. 600 [m, the weld penetration

- 202 - JAERI-Conf 99-009 was found to be deep. In case FL is 120 mm and the optical fiber of dia. 1000 pm, the width of the bead was found to be 2.2 mm, i.e., the greatest width.

1.3 Influence of Protective Gas and Nozzle of Optical Outlet Coupler When the laser beam reaches the material surface, plasma is formed causing the plume to be generated. Moreover, when the laser beam irradiates the material surface, metal vaporization reaction generated on the surface. Therefore, it has to be considered in the laser welding that such reaction is likely to cause some damage to the condenser. This reaction causes serious consideration on the pressure of the protective gas to be used, the diameter of the nozzle of the optical outlet coupler, the angle of incidence of the coupler and the distance between the material and the nozzle. Also, the protective gas and the plume phenomenon have a very close relationship in the welding process, and have great influence on the welding qualities. This laser welding experiment was conducted under the following conditions of the optical outlet coupler representing 50 LPM(Liter/Min.) of primary flowrate of helium (the flowrate of helium inside the nozzle), 12 mm of the distance between the material and the nozzle, and 7 mm of the nozzle diameter. When the secondary pressure of helium (gauge pressure), while helium was blown horizontally from the nozzle inlet, was increased from 0.3 atm to 1.4 atm, oxide zirconium was found to little cling to the condenser. However, when it exceeded 2 atm, the bead of the material surface was found to be rough due to the boiling phenomenon. Accordingly, it is judged that, in case primary flowrate of helium at the optical outlet coupler is 50LPM, the secondary pressure thereof shall be at least in the range of 1 atm to 1.4 atm.

2. Evaluation of Welding Quality 2.1 Microhardness Test The hardness test was conducted at the base metal, HAZ and the weld metal by Vickers hardness tester. Fig. 4 shows comparatively the results of the specimen welded by TIG and laser. In TIG and laser welded specimen, the hardness of the weld metal was found in the range of 180 to 210, and the hardness of HAZ between the weld metal and the base metal was found to be in the range of 160 to 180. The difference of the hardness of the weld metal between laser and TIG welded specimen was not so great, but in the hardness of HAZ, TIG welded specimen was found than laser welded specimen by about 10 to 20. And, in both TIG and laser welded specimen, the closer the test zone of the end cap sample was to the edge the higher the hardness was found to be a little higher than that of the cladding tube. It is, therefore, judged that the hardness was increased because the weld zone of the end cap

- 203 - JAERI-Conf 99-009 became abruptly cold from the overheating condition during the heat cycle. Also, the weld metal and HAZ area of laser welded specimen was found to be narrower, comparing with TIG welded specimen.

2.2 Tensile & Burst Test Table 2 shows comparatively yield strength, tensile strength and elongation obtained from tensile tests conducted in respect of respective geometrical configurations of TIG and laser welded specimen, i.e., A geometry (specimen with filler part) and B geometry (specimen without filler part). The tensile strength of both TIG and laser welded specimen were higher than that of the base metal. The tensile strength of TIG welded specimen was higher than that of laser welded specimen. However, the elongation of laser welded specimen tended to be a little higher than that of TIG welded specimen. And, there was little difference in yield strength and elongation between A and B geometry samples, and their tensile strengths were found to be similar. When the burst tests were examined, the ultimate burst elongation of laser welded specimen was found to be 36% in average, which was much higher than that of TIG welded specimen. Also, in the geometrical configuration of the welded zone, the mean value of ultimate burst elongation of A geometry sample was found to be high. Table 3 shows comparatively the ultimate burst strength and the ultimate burst elongation obtained from the seal burst test.

2.3 Microstructure Observation Since the weld zone is locally heated and cooled to the extent of its phase area or even beyond the phase area according to welding parameters, the weld zone experiences different phase transformations to have various microstructures.[4] It was observed that while the a grains in the microstructure of the base metal cladding tube were elongated longitudinally, the microstructure of base metal region of the end cap was of an irregular structure with the equiaxed a grains being recrystallized. While weld metal region of TIG welding appears to be very similar to quenched structure where prior grains typically grew greatly, weld metal region of laser welding appears to have a relatively small size of prior grains therein. This phenomenon seems to result from the fact that in case of laser welding, the absorbed heat energy was locally less than that of TIG welding, because the laser welding time was short and the cooling rates were very fast. Accordingly, weld metal region of the weld zone of the Zr-4 end cap appears to be of mixed structure, that is, the martensitic a' structure and the Widmanstatten a phase in the prior fi -grain are intermixed because of the relatively fast heating and cooling rates.

204 - JAERI-Conf 99-009

CONCLUSIONS The study was conducted to develop the Zircaloy-4 end cap welding, utilizing Nd:YAG laser system including the optical fiber transmission, and the performance of the welding is evaluated as follows. 1. From the result of examining the characteristics of the laser welding by optical fiber transmission, in case of the optical factor = 1.35, the weld penetration was found to be greater at FL = 95 mm than at FL = 120 mm. In case of the optical factor = 2.1, the bead width was found to be 1.8 mm at FL = 120 mm, which was wider than that of FL = 95 mm by 0.3 ~ 0.4 mm. 2. When the secondary pressure of helium (gauge pressure) at the optical outlet coupler during laser welding, is performed, was increased from 0.3 atm to 1.4 atm, oxide zirconium was found to little cling to the condenser. In case the primary flowrate of helium at the optical outlet coupler is 50LPM, the secondary pressure thereof shall be at least in the range of 1 atm to 1.4 atm. 3. When the Zircaloy-4 end cap weld zone was observed, laser welding zone has been smaller than TIG welding zone. The microstructures of the weld zone in both TIG and laser welded specimens, appeared to be of mixed structure, that is, the martensitic a' structure and the Widmanstatten a phase in the prior fi -grain were intermixed. 4. In the mechanical test of the Zircaloy-4 end cap weld zones, both processes were found to show good results, but the weld zone utilizing laser welding process was found to mostly have greater weld penetration than the one utilizing TIG welding, and further to have good weldabilities with fine grains.

REFERENCES [1] J. Saito, M. Shimizu : Development of Re-instrumentation Technology for Irradiated Fuel Rod, The 2nd Kaeri-Jaeri Joint Seminar on PIE Tech., KAERI- NEMAC /TR-32, (1995), pp. 125-135 [2] H. Sakai, H. Kawamura : New Apparatus of JMTR Hot Laboratory, Department of JMTR, The 2nd Kaeri-Jaeri Joint Seminar on PIE Tech., KAERI- NEMAC/TR-32, (1995), pp.65-77 [3] P. T. Truant : CANDU Fuel Performance & Power Reactor Experience, AECL-MISC- 250-3 Rev. 1(1983) [4] R. A. Holt: The Beta to Alpha Phase Transformation in Zircaloy-4, Journal of Nucl. Mat., 35 (1970), pp.322

- 205 JAERI-Conf 99-009

Table 1 Schedule of development of remote welding technology.

Phase Items 1998 1999 2000 2001 2002

- Fabrication of welding device I - Installation and cold test of laser _ welding device - In-cell demonstration test n - In-cell endcap welding performance

•J..-!*^--

Fig. 1 Photography of welding chamber using optical coupler.

- 206 - JAERI-Conf 99-009

Hot Cdh

Fig. 2 Schematic illustration of optical fiber delievery system in hot cell.

0.4 mm

(a) Macrostracture of TIG welding

0.4 mm

(b) Macrostructure of laser welding Fig. 3 Comparison of TIG and laser weldment.

- 207 - JAERI-Conf 99-009

WM 280 0.2 mr HAZ UBW O A GTAW • • 0*250 o 3 220 ©

190

M 160 o Weld center 130 Sheath <- -> End cap

5-4-3-2-101234 5 Distance from center of welds [mm]

Fig. 4 Microhardness variations along sheath-HAZ-endcap in TIG and laser welding. Table 2 Mechanical properties of TIG and laser welded specimens.

0.2% YS UTS %E Specimen Type Dimension (ksi) (ksi) in 50mm Each Ave. Each Ave. Each Ave.

62.5 78.4 37.2 A 65.5 62.9 80.1 78.4 35.6 37.1

TIG 13 08x12.24 60.8 76.8 38.5 welding (O.D) (1.D) 58.9 75.4 35.7 B 61.4 59.2 77.1 76.7 36.5 36.3 57.4 77.6 36.7 57.5 75.3 40.2 A 65.1 61.3 77.1 75.4 39.4 39.7 61.3 73.8 39.4 Laser welding 57.7 77.6 36.2 B 66.3 61.9 78.3 77.5 35.8 37.3 61.8 76.5 39.9

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Table 3 Burst properties of TIG and laser welded specimens.

UBS (MPa) UBE (%) Specimen Type Dimension Each Ave. Each Ave.

530 28.8 A 527 528 26.4 28.5

TIG welding 13.08x12.24 528 30.2 (O.D) (I.D) 532 28.9 B 524 527 27.5 28.2 525 28.1 524 39.9 A 526 526 36.2 37.8

Laser 528 37.2 welding 530 30.7 B 520 525 37.6 35.4 522 37.8

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2.11 SEM MODIFICATION AND SHIELDED GLOVE BOX

DESIGN FOR THE RADIOACTIVE MATERIAL

OBSERVATION

Ki-Seog Seo, Jeong-Hoe Ku, Kyoung-Sik Bang, Ju-Chan Lee, Gil Sung You, Dae-Seo Ku and Duck Kee Min Nuclear Fuel Cycle Development Korea Atomic Energy Research Institute P.O. Box 105, Yusong, Taejon, 305-600, Korea

ABSTRACT

The Scanning Electron Microscope(SEM) installation in the shielded glove box was performed for the first time at KAERI early in 1999. The SEM was modified for handling the radioactive materials. The shielded glove box will be used for SEM operation as well as storing and coating the specimen. This paper describes the SEM installation in the shielded glove box and the first experiences of the surface analysis of the radioactive materials.

INTRODUCTION

The hot cell in Post Irradiation Examination Facility (PIEF) at KAERI have only a metallography system for the analysis of microstructures. For more advanced research activity, the SEM could provide with the secondary electron, the backscattered electron mode and Energy Dispersive X-ray system (EDX) for the high magnification observation of microstructure and element analysis, respectively. The examination of radioactive fuels and irradiated materials by SEM will play an important role in providing data for basic mechanisms analysis involved in corrosion, radiation damage, fracture, etc.. The surface microstructures of materials are examined and analyzed by SEM for the determination of grain size, pore size and grain face fission gas bubble size. As the hot cells in PIEF have no space for SEM installation, a shielded glove box was required for a special purpose of SEM operation. Spent fuel specimen will be prepared in the hot cells with the same methods for metallography preparations such as the

- 210- JAERI-Conf 99-009 cutting, polishing etching and cleaning. In this paper, the modification criteria and contents of SEM are described firstly. PHILIPS XL-30 model was selected as a suitable equipment as this model needed a little modification for handling the radioactive materials. However, for the analyzing radioactive materials the SEM should be modified to prevent from the functional deterioration by the radiation effects. There are various types of shielding methods for SEM in foreign countries. Shielded SEM itself, the clamshell glove box type and shielded glove box type were compared mutually for our case. As shielded SEM is very expensive and clamshell type has complex structure, shielded glove box was decided as a best choice. The design requirements and contents of shielded glove box are described secondly in this paper.

MODIFICATION CRITERIA OF SEM

Comprehensive literature review related to a shielded SEM were at first conducted. The radioactivity of the specimens is ranged from 0.5 Sv/h to 1.26 Sv/h at contact(0.5 Sv/h by INEL, 1 Sv/h by ORNL, 0.72 ~ 1.26 Sv/h by SRL). As the SEM is to be applied to examine the radiation materials at the first time in Korea, our radiation criteria are decided to minimum 0.5 Sv/h at the specimen contact. And if the specimen is made from the nuclear spent fuel, its activity was estimated at 7.4 GBq. Its calculation was based on the values of the burn-up, the cooling time and the initial enrichment of 50 GWD/MTU, 3 years and 5 %, respectively. The weight of the spent fuel specimen is 0.17 gr. The modification criteria of our SEM were decided as followings ; 1) The shielding materials should protect all detectors and materials in the specimen chamber, in case their functions are reduced or lost by the radiation effects. 2) An electron gun and a control unit should be separated in order to install the electron gun only in the shielded glove box. 3) A specimen is easily installed or uninstalled on the stage of SEM by the manipulator. 4) A main function of the electron gun part shall be operated remotely for the use in the shielded glove box. Model XL-30 manufactured by PHILIPS was selected because they had the experiences for using their SEMs for the radioactive materials and their inside dimension of the stage chamber is very large. The large stage chamber has such advantage that the radioactive specimen is easily handled inside the chamber by the

manipulator. The filament of our SEM was adapted to LaB6 type to increase the period for maintenance. Highest resolution and magnification of XL-30 are 2.0 nm and

- 211- JAERI-Conf 99-009 x400,000, respectively. Analysis systems consist of a secondary electron detector, a backscattered electron detector and an energy dispersive X-ray system.

DESIGN REQUIREMENTS OF SHIELDED GLOVE BOX

For the application of SEM to the examination of irradiated nuclear fuel specimens, a shielded glove box was designed. It is important to determine proper shielding material and its thickness. It assumed that 6 specimens of the spent fuels were stored in the shielded glove box. Therefore, total radioactivity for the shielded glove box is 44 GBq. The shielding materials considered were the lead and the carbon steel, and its thickness was calculated by ANISN code. As the results of the shielding calculation, the thickness of the lead is about 8.5 cm and the steel is about 16.5 cm in accordance with the recommendation of ICRP-60, as shown in fig. 1. Because the shielded glove box should have various ports for the utility lines of the SEM and require a complex structure, the steel was decided as the shielding material for its convenience to fabricate the shielded glove box rather than the lead. The containment box shall be provided for the separation of the inner space of shielded glove box into two regions, so that the active zone for specimen examination is confined to avoid unnecessary contamination of the microscope and glove box inside. An exclusive transport cask is required in order to move the specimens from the preparation hot cell to the shielded glove box. For handling the specimen and the control of the SEM stage remotely, the manipulator and the lead glass are needed. And various ports and doors shall be provided for SEM maintenance and operation.

RESULTS AND DISCUSSION

1. SEM Modification for the Radioactive Material Observation The SEM has been modified according to the upper modification criteria. The acrylate conductor of the secondary electron detector was revised to the glass light conductor to lessen the radiation effects. The movements of the specimen stage were motorized in X, Y, Z directions and rotation. These capabilities make it possible to handle the specimen remotely outside the shielded glove box. However, the tilting movement is operated manually. The electrical cable, service lines and cooling water hose between the electron gun and the control unit was extended about 6-m length in order to install only the electron gun within the shielded glove box. Scan filtering system for our LaB6 filament was changed to the FEG filtering system to reduce the

- 212- JAERI-Conf 99-009 noise due to the long length of the electric lines. The open distance of the chamber door is extended from 20 cm to 30 cm so that the specimen is easily handled by using the manipulator, as shown in Fig. 2. The height of the electron gun is increased from 2 cm to about 5 cm in order to prevent the interference between the lower part of the electron gun and the bottom plate of the containment box. Al frame was provided outside the stage chamber so that SEM was connected to the containment box. EDX detector with super ultra thin window is added to the collimator. Its detecting range is Be(4) ~U(92). Instead of standard holder, a new special holder was fabricated. The SC7610 sputter coater system has two kinds of gold and carbon coater, as shown in fig 3. Each coater is comprised of three main parts: the cabinet assembly, the vacuum system and the chamber. The vacuum system of them must be modified to coat the radioactive materials. The items were modified as follows: The another cabinet is fabricated for the vacuum system and the chambers to be installed within the shielded glove box. The service connection cables that connect from the vacuum system to the cabinet assembly are extended to about 4 m.

2. Shielded Glove Box Design The shielded glove box consists of containment box, shielding walls, lead glass, manipulators, maintenance doors and specimen cask adapters, etc. The overall size of the glove box is 2.07 m wide, 2.17 m depth and 2.62 m high. The walls are made of carbon steel plates with a thickness of 170 cm. The front, sidewalls and roof panels are fixed by interconnecting with bolts and joint panels whereas the rear wall is movable for the easy access for maintenance. Each shield wall panel is made of two layers without seam and fixed together by bolts. The lead glass and manipulators were installed in the front shielding wall, so that the specimens are remotely handled from the specimen loading to the SEM specimen door opening with good visibility. The specimens are transferred from the hot cell to the containment box using specially designed specimen cask and are picked up using manipulator. At the outside of right sidewall, the cask adapter was installed to transfer specimens between the glove box and hot cell. A schematic drawing of the glove box is shown in Fig. 4 and Fig. 5. The walls of the containment box are made of reinforced glasses with aluminum frame to ensure the sufficient illumination and visibility. The jointing interface of containment box and SEM is connected by folding rubber, so that it can accommodate the lifting movement of SEM specimen table. HEP A filters at the inlet and outlet of containment box, and manometers were installed to maintain the negative pressure of

- 213- JAERI-Conf 99-009 the inside cavity of containment box so that no contamination materials can escape. The lights are positioned at the inside top of the roof panel. Three doors were prepared to aid proper maintenance works. Rear door can be opened fully by electrically driven motor for the easy installation of SEM. Left door with 600 mm width is used for maintenance of SEM specimen stage using gloves because the specimen stage is located inside of the containment box. The front door is used for normal checking of vacuum pump operation and adjusting cooling water level. Specimen storage rack with shield was prepared inside the containment box so that the maintenance can be made safely despite of the highly radioactive specimens.

REFERENCES

1. PNL, "Shielded Analytical Instruments for Characterization of Highly Radioactive Materials", PNL-5862, 1986. 2. BNL, " A Fully Shielded & Analytical Scanning Electron Microscope for the Examination of Radioactive Materials", EMAG-91, 1991 3. INEL, "Operation of a Scanning Electron Microscope in a Hot Cell", DE88-006775, 1987. 4. ORNL, "Scanning Electron Microscope Facility for Examination of Radioactive Materials", ORNL/TM-9451,1985.

- 214- Fig. 1 Thickness of Shielding Material According to Dose Rate.

Increasing the Height of the Electron Gun Extension of service lines

Fig. 2 Modification of XL-30 Electron Gun Fig. 3 Modification of Sputter Coater Fig. 4 Section View of the Shielded Glove Box

Fig. 5 Plane View of the Shielded Glove Box JAERI-Conf 99-009

SESSION 3

EVALUATION OF PIE DATA

IRRADIATION EFFECTS OF IN-CORE COMPONENT CHAIRS : E.-K.Kim (KAERI) and T.Tsukada (JAERI)

FUNDAMENTAL BEHAVIOR OF DRIVER FUELS CHAIRS : K.Ogata (NFD) and T.Maruyama (JNC)

R&D FOR THE NEXT DECADE AND USERS' REQUIREMENTS FOR PIE CHAIRS : T.Shikama (Tohoku Univ.) and Y.-S. Kim (Hanyang Univ.)

- 217- This is a blank page. JP9950642 JAERI-Conf 99-009 3.1 DETECTION OF DEFECTS IN CONTROL RODS BY EDDY CURRENT EXAMINATION

Dae-Seo KOO, Jeong-Hoe KU, Duck-Kee MIN, Ro Seung-GY, Young-Sang JOO and Yoon Kyu PARK*

Department of Spent Fuel Examination Technology Korea Atomic Energy Research Institute P.O.Box 105, Yusong, Taejon, Korea

ABSTRACT

To detect the defects of control rods in a reactor, a standard specimen including external defects, internal defects, and through-hole defects is fabricated. The eddy current signals of these defects are stored, analyzed on a PC by a program developed to acquire data of eddy currents. The optimum frequency for detecting defects of the control rods is 200kHz. The defect location, and defect shape of the cladding in the control rods are detected by analyzing the impedance phase of the eddy current. It is confirmed that the defects in hafnium of control rods can be detected.

INTRODUCTION

The control rods, which shut down or control the power of the reactor, must be free from defects for normal operation. In case defects occur in the control rods during the operation of the reactor, it is necessary to swiftly utilize the technology for conducting integrity tests, defect detection and clarification of the cause[l~3]. In this paper, the standard specimen, including external, internal, and through-hole defects is fabricated for detecting defects in control rods, and

* : Nuclear Environment Technology Institute

- 219 JAERI-Conf 99-009 the characteristics of the eddy currents of the standard specimen are analyzed by developing a program for data acquisition/data analysis of eddy currents. The possibility of identifying the defect location, and defect type in the cladding of the control rods and defects of hafnium in the control rods is confirmed by analyzing the impedance phase and impedance amplitude using eddy current examinations[4~5].

EXPERIMENT

The main ECT(eddy current test) equipment, DEFOSCOPE, is made by Intercontrole company in France and it can continuously change from 1kHz to 1MHz. The eddy current flows into the specimen as a result of exciting the ECT system, which includes an differential encircling coil, with an optimum frequency. The eddy current is amplified, displayed on CRT by adjusting the impedance phase of the amplified eddy current, impedance amplitude of amplified eddy current. This eddy current consists of a resistance and a reactance component, and it is stored, and analyzed using a PC through an A/D(analog to digital) converter which uses data acquisition and data analysis. The A/D converter has a resolution of 12 bits and the program for data acquisition and data analysis programmed using C language. The step motor device for moving the control rods in a vertical direction or rotational direction is fabricated and it is possible to continuously confirm the location of the control rods. Fig. 1 indicates the differential encircling probe which is used for eddy current examinations. The standard specimen including external (0.2mm(depth) x0.2mm(width)x3.0mm(length)),internal(0.2mm(depth)x0.2mm(width)x 3.Omm(length)), through-hole (0.5mm in diameter) defects is fabricated for determining the optimum conditions of an eddy current examination. Fig. 2 shows the impedance phase, and impedance amplitude due to standard defects at an optimum frequency of 200kHz. The impedance phase, and impedance amplitude due to defect type, and defect size are distinguishable. Therefore, the determination of the impedance phase of an eddy current of conducting material enables the detection of defect types.

- 220 - JAERI-Conf 99-009

inside of Hotcetl

Control Rod with Coil 2 Artificial Notches

Coil 1 Radiation Shielding Wall

Fig, 1. Schematic Diagram of Probe and Standard Specimen.

STANDARD RIG NOTCHES BY EDM

OUTER NOTCH

Resistance

OUTER NOTCH(M) : 0,2(0) X 0.2(W X 3.0tU IWER HOTCH(H) : O.ZiD) X 0.2«) X 3.0tU THROUGH H«£(M) : 0.5

Fig. 2. Eddy Cument Signals of Artificial Notches in a Standard Rig.

- 221 - JAERI-Conf 99-009

RESULT AND DISCUSSION

It is reported that the impedance phase of an external defect in conducting material has the range of 10 — 35°, that of an internal defect the range of 35 — 55°, and that of a through-hole defect has the range of 55~165°[6~8]. The characteristics of eddy current from the fabricated standard specimen, including external, internal and through-hole defects, are distinguishable at an optimum frequency of 200kHz. The defects of the control rod A, and control rod B in the reactor are detected, and analyzed using this optimum technique of eddy current examination. Fig. 3 and 4 indicate the eddy current signals of two local bulges,

hafnium-hafnium interface, hafnium-B4C interface, wear and a scratch as result of the eddy current examination located 789mm, 881mm, 970mm, 1049mm, 1258mm and 1493mm from the bottom end of the control rod A, respectively. Fig. 5 indicates an eddy current signal of a hafnium-hafnium interface at 390mm from the bottom end of control rod B. The defect location and defect type on the control rods can be detected by analyzing the impedance phase, and impedance amplitude and the possibility of detecting the defects of hafnium in the control rods is confirmed.

CONCLUSIONS

1. The characteristics of an eddy current for a standard specimen including external, internal and through-hole defects are distinguishable due to defect type, and defect size, at an optimum frequency of 200kHz. 2. The eddy current signals of two local bulges, scratch, hafnium-hafnium

interface, hafnium-B4C interface and of wear on control rods were detected. 3. The possibility for detecting defects in the cladding of control rods and for detecting defects of hafnium in control rods using eddy current examination is confirmed.

- 222 - JAERI-Conf 99-009

LOCAL BULGE

itf .

-i - H I] 1 \- Resistance

(a)

V 'fl;

UJ -2- I 2 +

FISGUEKCY 200KHz

900 SOD 7DD 620 DISTANCE FROM BOTTOM!™)

(b)

Fi«. 3. Eddy Current Signals of Defective Control Rod A, (a) Eddy Current Signal in Impedance Plane, (b) Resistance and Reactance of Eddy Current in Defective Control Rod A,

- 223 - JAERI-Conf 99-009

toco 1200 1400 1600 1600

DISTANCE FROM BOTTOM(am)

(a)

Fig. 4. Eddy Current Signals of Defective Control Rod A. (a) Resistance and Reactance of Eddy Current in Defective Control Rod A. (b) Eddy Current Signal in Impedance Plane.

- 224 - JAERI-Conf 99-009

(a)

4- j 2- 1 n • -2- 3 -4 *Hf- HflMTERFACE i ij 2-

-2 -4- If FREQUENCE 2QGKHi

150 300 490 DISTANCE PROM BOTTOMimn) (b)

Fig. 5. Eddy Current Signals of Control Rod B. (a) An Eddy Current Signal in Impedance Plane, (b) Resistance and Reactance of an Eddy Current in Control Rod B,

- 225 - JAERI-Conf 99-009

REFERENCES

[1] H. W. Keller et al., " Development of Hafnium and Comparison with Other Pressurized Water Reactor Control Rod Material," Nucl. Tech., Vol. 59, 576(1982). [2] W. J. Johnson to C. E. Rossi Letter Number NS-NRC-88-3389 dated December 19, 1988 entitled, " Summary of Full Length Hafnium RCCA Anomaly Update," (1988). [3] K. S. Choi and I. K. Kim," Development of a Computer Program for Drop Time and Impact Velocity of the Rod Cluster Control Assembly," J. of the Korean Nuclear Society Vol. 26, No. 2, 197(1994). [4] R. D. Phipps et al., " Eddy-Current Examination of Irradiated Fuel Elements at the Hot Fuel Examination Facility," Proc. 25th Conference on Remote Systems Techno logy (1977), pp. 245 — 250. [5] J. H. Flora et al., " Nondestructive Examination of Irradiated Fuel Rods using Encircling and Probe Eddy-Current Systems," Proc. 25th Conference on Remote Systems Techno logy (1977), pp. 264—271. [6] T. R. Crowe, "Calibration of Eddy Current Systems with Simulated Signals," Mat. Eval. Vol. 35, 59(1977). [7] A. P. Steinberg et al., "Determining Crack Depth in a high-Strength Steel Cylinder using Magnetic Perturbation," Mat. Eval. Vol. 40, 288(1982). [8] J. B. Hallett, G. V. Drunen and V. S. Cecco, "An Eddy Current Probe for Separating Defects from Resistivity Variations in Zirconium Alloy Tubes," Mat. Eval. Vol. 42, 1276(1984).

- 226 - JP9950643 JAERI-Conf 99-009

3.2 Life Time Estimation for Irradiation Assisted Mechanical

Cracking of PWR RCCA Rodlets

TakanoriMATSUOKA* • YouicirirouYAMAGUCffl*

* Experiment Department, Nuclear Development Corporation 622-12 Funaishikawa, Tbkaimura, Ibaraki 391-1111, JAPAN

Abstract

Intergranular cracks of cladding tubes had been observed at the tips of the rodlets of PWR rod cluster control assemblies (RCCAs). Because RCCAs were important core components, an investigation was carried out to estimate their service lifetime. The reviews on their mechanism and the life time estimation are shown in this paper. The summaries are as follows. (l)The mechanism of the intergranular crack of the cladding tube was not IASCC but irradiation assisted mechanical cracking (IAMC) caused by an increase in hoop strain due to the swelling of the absorber and a decrease in elongation due to neutron irradiation. (2)The crack initiation limit of cylindrical shells made of low ductile material and subjected to internal pressure was determined in relation to the uniform strain of the material and was in accordance with that of the RCCA rodlets in an actual plant. (3)From the above investigation, the method of estimating the lifetime and countermeasures for its extension were obtained.

Introduction

The tips of the rodlets in rod cluster control assemblies (RCCAs) are exposed to extremely high neutron fluence in fuel assemblies. Since high neutron fluence causes degradation of the cladding tube material (Type 304 stainless steel) and swelling of the neutron absorber (80%Ag-15%In-5%Cd Alloy), the integrity of the RCCA may be affected. On-site rodlet outer diameter measurements and hot cell examinations of typical rodlet tips were carried out for the RCCAs of a PWR plant (2-Loop, 500MWe, Fuel Type

- 227 - JAERI-Conf 99-009

14 x 14)after 10 cycles. During the post irradiation examination an intergranular crack of a cladding tube had been observed near the tip.a) The cause of the intergranular crack was investigated that its mechanism was not IASCC but irradiation assisted mechanical cracking (IAMC) caused by an increase in hoop strain due to the swelling of the absorber at a very slow strain rate and a decrease in elongation due to neutron irradiation. ®0)M> Then the crack initiation limit was estimated by considering the decrease of the uniform strain of Hie cladding tube and the increase of the outer diameter of the control rods. From the results, a lifetime estimation method and countermeasures for cladding tube cracking were obtained. ® The reviews are carried out on IAMC of PWR RCCA rodlets and their life time estimation according to the references from (1) to (4).

Post Irradiation Examination

1. On-Site Measurements The outer diameters of control rods were measured by cantilever-type springs on which strain gauges were attached. The equipment was calibrated using a standard rod. This equipment could make measurements at four axial locations on each rodlet and could simultaneously measure all the rodlets in one RCCA The results of the diameter changes are shown in Fig.l. The maximum outer diameter change was approximately 0.1mm(about 1% increase of the cladding outer diameter). Although there is considerable scatter in the changes in the outer diameters of the rods in one RCCA, the range of values is almost equal to the tolerance for the gap between the cladding tube inner diameter and absorber outer diameter. Figure 1 also shows the relationship between the change in outer diameter and neutron fluence, in which a higher fluence results in a larger change of outer diameter.

2. Selection of Segments hi order to investigate the degradation of cladding tube material and irradiation induced swelling of the absorber, the RCCA which had been exposed to the highest fluence of 1.2 X 1026n/m2, E>lMeV, was subjected to post irradiation examination. Two rodlets were selected for examination. Rodlet No. 1 : This rodlet had the largest outer diameter increase. Segment A : A sample of the middle section, where the neutron exposure is negligible(for reference material properties without neutron irradiation) Segment B : A sample of a rodlet tip (for swelling investigation) Rodlet No. 2 : This rodlet had the smallest outer diameter increase.

- 228 - JAERI-Conf 99-009

Segment C : Asample of a rodlet tip(for investigation of cladding tube degradation) The locations of the segments are shown in Fig. 2. These segments were cut out at the site and transferred to the hot laboratory.

3. Examination of the absorber 3.1 Changes in the Outer Diameter of the Absorber. The absorber outer diameters of segments A, B and C were measured using a micrometer to obtain the relationship between the increase in outer diameter and the corresponding neutron fluence. The control rod outer diameters at various locations on segment C were calculated by adding twice the cladding tube thickness to the measured outer diameter of the absorber and compared with the on-site control rod outer diameter measurements. As shown in Fig.3 the results agree closely with each other. The distribution of neutron fluence along the examined rodlets is shown in Pig.4. The neutron fluence decreases rapidly over a short distance from the rodlet tip on account of the axial neutron flux distribution in the core. The neutron fluence in Fig.4 is the value calculated from the core design of the plant concerned. The changes in the outer diameter of the absorbers (segments B and C) were obtained by subtracting the measured diameter of segment A from those of segments B and C. The relationship between the change in absorber outer diameter and neutron fluence is shown in Fig.5, which shows a linear correlation. 3.2 Density of the Absorber The density of the absorbers was measured by the liquid immersion method at the tip and middle part of the control rods. The results are shown in Fig.6. Densities at the control rod tip for segments B and C are lower than the original value and the decrease is in proportion to the irradiation. On the other hand, segment A which was exposed to low irradiation shows no change.

4. Examination of the Cladding Tube 4.1 Characteristics of the Cladding Tube Material Small test specimens, shown in Fig.7, were taken from the cladding tubes of segments A, B and C, and tensile tests were carried out at room temperature and at 320^ which is the actual reactor coolant temperature of the plant. As shown in Table 1, the results for segment A, which was exposed to a very low fluence, were close to those given in the inspection certificate. However, the test results for segments B and C were different from the inspection certificate data and showed significant irradiation hardening. At 320t:, the yield strength(0.2% oflset)was 800—9 lOMPa, the tensile strength was 950~ 1050MPa, the fracture strain was 5.3~~6.0%, and the uniform strain was 1.4~1.5 %.

- 229 - JAERI-Conf 99-009

Since only a limited amount of irradiated cladding tube material was available, the tensile tests of unirradiated cladding tube material were carried out on both tubular specimens and the above-mentioned small specimens shown in Fig.7 in order to examine the effects of size and shape and to determine the tensile properties of unirradiated material. As shown in Table 2, the tensile properties obtained from small-size specimens are in good agreement with those obtained from the tubular specimens. 4.2 Investigation oftiie Cracked Tip In segment B taken from the tip of Eodlet No.l, which had shown the largest outer diameter increase, an axial crack was observed from 55mm above the rodlet tip to the cut-off position. Therefore, metallographic inspection of the cladding tube material and SEM observation oftiie fracture surface were carried out for the cracked cladding. The typical metallography of the cracked region in segment B is shown in Fig.8. The crack seemed to be an intergranular one and no other cracks were observed The cracked region was opened forcibly to expose the crack surface. The crack surface and deliberately fractured surface were observed visually and by SEM. The results are shown in Fig.9. Because of crud produced in the high temperature water of the reactor, the color of the crack surface was black, which was quite different from the silver white of the deliberately fractured surface. In addition, the length of the inner surface of the crack was slightly longer than that of the outer surface. Therefore, the crack was considered to have been initiated at the inner surface. As shown in Fig. 10, the fracture surface was completely intergranular, but both intergranular and transgranular surfaces were observed in the deliberately fractured region in the SEM investigations. In the fracture surface of the tensile specimen tested at 3201 at a low strain rate of 6 X lO^/s, a small percentage of the fracture surface was observed to be intergranular as shown in Fig. 11. Sipush et aL' s result ®® is shown in Table 3. Fully intergramilar cracks would have been observed on the fracture surface if the tests had been carried out at very low strain rates of 10"10 to 10u/s, which is the assumed strain rate due to swelling of the absorber by neutron irradiation in the actual plant. From Table 3, uniform strain, which corresponds to the necking point, is independent of the strain rate although the proportion of intergranular fracturing of the surface is dependent on the strain rate. For segments A and C, dye penetrant tests were carried out and no indication of cracks was observed. 4.3 Hydrogen Content It is evident that an intergranular crack is induced by the very slow extension strain rate but the mechanism which causes tile intergranular crack is not clear. To help the investigation, the hydrogen contents of the cladding tubes were measured.

- 230 - JAERI-Conf 99-009

The results are shown in Table 4. Specimens were taken from the tensile test specimens as shown in Table 4 and analyzed for hydrogen content by the hot melt gas stripping method using a melting temperature of between 2200t and 2400°C. The hydrogen content of an unirradiated dadding tube is also shown in Table 4. The value is dose to that of segment A, which was subjected to a low irradiation dose. Pig. 12 shows the hydrogen content of irradiated Type 304 SS as a function of fast neutron fluence (E>lMeV). The condusion from the BWR measurements was that the hydrogen content was independent of both fast neutron fluence and flux. CT But the hydrogen content seemed to increase rapidly above a fluence of lO2^^2 in Pig. 12, although the measured values were scattered over a wide range. It was possible that the hydrogen content did depend on neutron fluence and further studies would be needed to determine the relationship. Therefore the hydrogen content seemed to be one of the causes of inducing intergranular cracks in a cladding tube at very low strain rates of 1010 to 10u/s.

Investigation of the Crack Initiation Mechanism

1. Definitions of the Crack Initiation Mechanism Because mechanisms of cracks induced by material degradation due to neutron irradiation in nudear reactors are not dearly denned up to the present, their definitions are settled as follows. (1) The whole cracks induced by material degradation due to neutron irradiation are defined as irradiation assisted crackings (IAC) (2) Cracks induced by stress corrosion in IAC are defined as irradiation assisted stress corrosion crackings (IASCC) (3) Cracks induced mechanically in IAC are denned as irradiation assisted mechanical crackings (IAMC) Figure 13 shows a comparison between IAMC and IASCC. IAMC is initiated when the strain exceeds the crack initiation strain limit without any relationship to the elapsed time. But IASCC of bolts and welding parts is initiated in a corrosive atmosphere a long time after stress corrosion cracking susceptibility has started.

2. Mechanical Crack Initiation Limit It is very important to obtain crack initiation strain limits for IAMC since investigation whether the crack is mechanical one or not depends on them. Cooper®, Svensson®, as well as Eihara and Fujitaa(? investigated the fracture strain of

- 231 - JAERI-Conf 99-009 a cylindrical shell made of ductile material and subjected to internal pressure. Though Type 304 SS was a ductile material, the material of the cladding tube had to be treated as a low ductility material in order to obtain its crack initiating limit because its ductility was reduced by neutron irradiation. The crack initiation limit of a dadding tube was given as follows by considering the cladding tube to be a pressure vessel.®

E^S^+W £^ (1) where e „ : Elastic component of uniform strain £ ^ : Plastic component of uniform strain

3. Crack Initiation Mechanism ofRCCARodlets Irradiation assisted stress corrosion cracking QASCC) might be the cause of an intergranular crack of a dadding tube because the metal was subjected to a high neutron fluence of up to 1026n/m2. However the crack was single and was initiated at the inner surface of the cladding tube(1), also Sipush et aL got intergranular fracture surface during tensile tests of irradiated cladding tubes at a very strain rate in an argon gas atmosphere®. This shows that the mechanism of the intergranular crack in the cladding tube is not IASCC but irradiation assisted mechanical cracking (lAMC) caused by an increase in hoop strain due to the swelling of the absorber at a very slow strain rate and decrease in elongation due to neutron irradiation. Since a crack had been found in the cladding tube tip in the hot laboratory, all of the remaining 14 rodlet tips of the RCCA with the highest neutron fluence(1.2 X lO^n/m2, E>lMeV)and all 16 rodlet tips of another RCCA with a neutron fluence of 0.7 X 102Sn/m2, E>lMeY were examined on site using a fiber scope. A single axial crack was found in two rodlets of the first RCCA Thus a total of 3 rodlets were found to have a crack.(1) On the other hand, no cracks were found in the second RCCA The increases in the outer diameter of the two cracked rodlets observed on site using a fiber scope were 80 IL m and 83 \i m and that of the cracked rodlet found during the hot cell examination was 88 ft vex. Cracks were observed only in control rods which had outer diameter increases of 80 p. m or more in the cold condition. The increase in outer diameter of 80 n m corresponds to 0.7% strain of the dadding tube. The difference in the thermal expansion of the absorber and the dadding tube is approximately 0.3%. ® The dadding tube strains of the cracked rodlets are therefore estimated to be more than 1.0%. Prom the tensile test of an irradiated cladding tube, uniform strain at 320t> is 1.4% and f ue is equal to 0.6% and £ ^ is equal to 0.8%. Then the critical strain for crack initiation is estimated to be 1.0% from Eq. (1) Since the measured changes in outer

- 232 - JAERI-Conf 99-009 diameter agree well with the strain at crack initiation obtained from the tensile test, cracking is considered to be initiated when the increase in outer diameter is approximately 80 // m (0.7%) or more in the cold condition. As shown in Fig.l, the neutron fluence at the intersection of the dashed line corresponding to a conservative estimate of the increase in the cladding tube outer diameter, and the chain dotted line that corresponds to the critical increase in outer diameter for crack initiation, is approximately0.8 X 10asn/m2,(E>lMeV).® The neutron fluence (E>0.625eV) is convenient for practical fluence management of RCCAs, since a 0.625eV energy cut-off is usually used in PWR core calculations. The neutron fluence(E>0.625eV)is approximately four times the neutron fluence(E>lMeV), therefore, 3 X 1026n/m2(E>0.625ey)corresponds to the critical neutron fluence for axial crack initiation.

life Time Estimation

1. Life Time Estimation Method The mechanism of the intergranular cracking of the cladding tube was irradiation assisted mechanical cracking (lAMC) caused by an increase in hoop strain due to the swelling of the absorber at a very slow strain rate and decrease in elongation due to neutron irradiation. The life time was determined by the time at which the strain of the cladding tube induced by absorber swelling exceeds the crack initiation limit which is given by Eq.(l) Because the effect of slumping of the absorber was negligible, the gap between the cladding tube and the absorber was the essential factor for determining the point at which the outer diameter started to increase after the gap had been reduced to zero due to absorber swelling. This means that if the gap is larger, it takes a longer time before the outer diameter starts to increase.® Cladding tube cracking in RCCA rodlets might not affect the performance of an RCCA, since only a single axial crack had been found and the silver-mdiurn-cadmium alloy used for the absorber was very stable when exposed to high-temperature water. However, the method of estimating the life time for cladding tube cracking of RCCA rodlets has been obtained from the above mentioned investigation.

2. Estimation of the Increase in Cladding TUbe Outer Diameter The mechanism of cracking and the critical increase in the outer diameter are shown quantitatively in Fig.l.® Since the change in the control rod outer diameter corresponds to the change in the absorber outer diameter shown in Fig.5, the control rod

- 233 - JAERI-Conf 99-009 outer diameter is considered to increase linearly with neutron fluence. The solid line in Pig. 1 shows the change in rodlet diameter with neutron fluence and is the mean value of the rodlets of the five RCCAs with a high fluence. On the other hand, the dashed line shows the maximum change in control rod outer diameter estimated from the change in absorber diameter shown in Pig.5 and ignoring the initial gap between the cladding tube and the absorber under hot conditions. This gap is a little less than the design gap in the cold condition. This dashed line envelops the on-site data and has a similar slope to that of the mean line. Therefore, it is considered that this dashed line gives a conservative estimate of the increase in the cladding tube outer diameter.

3. Effect of Hie Gap between the Cladding Tbbe and Absorber on Life Time The gap between the cladding tube and absorber is the essential factor for determining the point at which the outer diameter starts to increase after the gap has been reduced to zero due to absorber swelling. The effect of the gap between the cladding tube and the absorber is shown in Fig. 14 using the relationship between change in outer diameter and neutron fluence.® The critical neutron fluence that corresponds to crack initiation is conservatively estimated to be 3 X 1026n/tn2(E>0.625ey) for the conventional RCCA rodlets. Pig. 14 can also be used to estimate the life time of RCCAs with an increased gap between the cladding tube and the absorber.

Conclusions

The authors showed the review on irradiation assisted mechanical cracking of PWR RCCA rodlets and their life time estimation. The conclusions are as follows.

(l)The mechanism of the intergranular cracks in the cladding tube was not IASCC but irradiation assisted mechanical cracking(lAMC) caused by an increase in hoop strain due to the swelling of the absorber at a very slow strain rate and decrease in elongation due to neutron irradiation. (2)The cladding tube crack initiation limit for PWR RCCA rodlets due to absorber swelling was investigated by considering the tube as a pressurized cylindrical shell and this agrees well with the outer diameter increases measured at site. (3)The critical neutron fluence for axial crack initiation was approximately 0.8 X 1026n/m2(E>lMeV) or 3 X 1026n/m2(E>0.625eV). The latter was an appropriate criterion in terms of actual core management. Axial cracking in an RCCA rodlet could be prevented if RCCAs were replaced before the total neutron fluence reaches

- 234 - JAERI-Conf 99-009

the above value. (4)Reducing the outer diameter of the absorber at the tip or increasing the gap between the cladding tube and the absorber, could be adopted as a method of getting the required RCCAlife time.

References

(1 )Matsuoka,T., Yonezawa/T., Tbmimatsu,M., Mon^M., Myojin,H., Sasaki,Y, Ootani,M, NagataX Intergranular Cracking in Cladding Tube of PWR RCCA Rodlets, JSME International Journal VoL38 No.4-A, p515-523 (1995). ( 2 )Matsuoka,T., MoriJVL, Nakamura,K, Myojin, H., Nagata, T., Crack Initiating limit for Cladding Tubes of PWR RCCA Rodlets Subject to Absorber Swelling, JSME International Journal VoL39 No.4-A, p555-564 (1996). (3 )Matsuoka,T., Yonezawa,T., NakamuraJKL, MurakamiJL, Shimizu,J., Nagata,T., life Time Estimation for Cladding Tube Cracking Causes by Absorber Swelling of PWR RCCA Rodlets, AESJ Journal of Nuclear Science and Technology VoL35, No.8, p564-578(1998) ( 4 )Matsuoka,T, Yamaguchi,Y., Yonezawa,T, NakamuraJL, FukudaJR., Shiraishi,S., Irradiation Assisted Cracking of RCCA Rodlets and Experimental Techniques for their Improvement, Fontevraud IV International Symposium Proceedings, p221- 235(1998) ( 5 )Manahan,MP., Kohli,R, Santucci, J., Sipush,P. and Harris,R.L., Irradiation-Assisted Cracking of Control Rod Cladding, Trans, of the 9th SMiRTC, p75-85, (1987). ( 6 )Sipush P.J., Woodcock,J. and ChickeringJl.W., lifetime of PWR Silver-Indium- Cadmium Control Rods, EPRI-NP-4512, (1986). ( 7) Jacobs, A J., Hydrogen Buildup in Irradiated Type-304 Stainless SteeUnfluence of Radiation on Material Properties: 13th International Symposium(Pert II), ASTM STP956, p239-244(1987). ( 8) Cooper, WE., The Significance of the Tensile Test to Pressure Vessel Design, Welding Journal 36, p49-s-56-s, (1957). (9) SvenssonJN.L., The Bursting Pressure of (Cylindrical and Spherical Vessels, Journal of Applied Mechanics 25, p89-96, (1958).

(10)KihararH. and FujitaX Ductility Strength,(in Japanese) JHPI, Vol.2, No.6, pl7-24, (1964).

- 235 - JAERI-Conf 99-009

Tablei Results of tensile tests of irradiated cladding tube material

Test Condition Yield Tensile Uniform Fracture Fluence Segment Strength Strength Strain Strain /Vcm\ \ Test Temp. Strain Rate (MPa) CMPa) (%) \E > lMeVJ CC) (1/sec) (%)

Room A 6 x 10"s 687 829 17 33 5x 1013 Temp.

A 320 6xlO-6 613 734 6.3 11 2x 1014

B 320 6X10'6 908 1032 1.4 5.9 9.0 x 1021

B 320 6 x 10-6 881 1046 1.5 6.0 1.1 x 1022

C 320 6 x lO*6 799 953 1.4 5.4 8.3 xlO21

C 320 6 x 10-5 868 1010 1.4 5.3 a3 x 1021

C 320 6 x 10-6 868 981 1.4 5.4 1.1 x 1022

Inspection Room — 616 745 — 38 — Certificate Temp.

Table2 Results of tensile tests for unirradiated cladding tubes

Test Condition Strain Rate Strain Rate Yield Tensile Fracture Uniform Specimen Temp. up to from Yield Strength Strength Strain Strain Yield Strength to (MPa) (MPa) (K) (X) (1C) Strength Fracture (1/s) (1/8) — 864 44 38 1.7x10' 1.7X10* Room — 804 47 40 Temp. — 782 47 40 Tubular 1.7x10" 1.7x10"' Specimen — 769 49 42 — 629 18 13 320 1.7x10" 1.7x10" — 627 17 13 612 791 49 42 6X10"' 6X10- Room 629 795 49 39 Temp. 607 777 50 30 6x10" 6x10" Small 628 777 44 36 Specimen 509 599 16 11 6X10"1 6x10" 486 591 18 11 320 491 571 22 14 6x10" 6x10" 497 625 20 13

- 236- JAERI-Conf 99-009

Table 3 Results of tensile tests for irradiated Type 304SS cladding tubes fromRefs.(5) and

Test condition Intergranular ,,. ,, . ., Tensile Uniform FVacture Fluence Specimen TT. .. Yield strength ...... ,2 No. Test temp. Strain rate (MPa) Fractur(96) e ,,,„ x strengt(MPa)h strain strai(96)n (\E> n/mlMeV , \/

C-l 315 5.0 x 10"4 0 909 924 3.3 8.0 6 C-2 315 1.0 X 10" 3-4 936 944 1.6 9.3 5 X 1025 C-3 315 2.0 X 10~T 15-20 tt 865 tt 4.3 C-4 315 1.0 x 10~8 30-35 tt 848 2.6 6.8 6 D-l 315 1.0 x KT 763 792 2.7 15.0 4 x 10"

* The atmosphere was argon gas for all tests reported here. '* These data cannot be reported due to uncertainty in the load-time record.

Table 4 Hydrogen content of cladding tubes

Segment Hydrogen contents Fluence (wt. ppm) (n/mV£>lMeV) 13 0.5 x 1018 A 11 2 x 10" 229 0.9 x 1026 B 48 1.1 x 1026

79 0.8 x 1026 37 C 132 26 1.1 x 10 11 Unirradiated 8 0 cladding tube

Tensile Test Specimen

Test Specimen (5mm 0)

- 237 - JAERI-Conf 99-009

Estimated Maximum Control Rod 1.5 A Defective Rodlet 150 • Outer Diameter Increase Max.

Mean e.= t.+ e-/ [I/Thermal Expansion's 1-0 * 100 Min. Kabout 03% ) Mean Line for about 0.7% V Increase in Outer Diameter of 5 RCCAs I with Highest Undamaged* Fluence 50 0.5 —Rodlet Na2 Undamaged ! o Sample RCCA for PIE O

-50 -0.5 SS Fiber Scope Inspection was Performed for 32 Rodlets

-100 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Neutron Fluence at Rodlet Tip (xl0"n/m, E > lMeV)

Fig. 1 The mechanism of cracking and the critical increase in the outer diameter of a rodlet

Control Rod

Rodlet 1 Rodlet 2 (Max Diameter Increase) (Min. Diameter Increase)

Top End Plug

Cladding (Type304SS)

Neutron Absorber (Ag-In-Cd Alloy)\

Bottom End Plug

Fig. 2 RCCA rodlet configuration and location of segments taken from rodlets

- 238 - JAERI-Conf 99-009

• : On Site Results

A : Results Calculated from .11.05 Measured Absorber Diameters I Measured Absorber Diameter | |_ + 2x (Cladding Thickness) J

11.00 Q.2

1 10.95 "8 0i

10.90 100 200 300

Distance from Control Rod Tip (mm)

Fig.3 Comparison of rodiet outer diameters obtained by measurement of absorber diameter with those measured during the on-site examination

Cladding (Type304SS) Absorber (Ag-In-Cd Alloy)

Ci ll{;i;i;ii;;;;i;;;;;i;i;;:i;;;:;;;^i;;i;i;i;Miii;i:i:i-n:;;ii-;;:;i:i;!;;;;;::i;i:;i;

(xl0"n/m')

S i—t A © I

0 100 200 300

Distance from Control Rod Tip (ram)

Fig. 4 Relationship between distance from the tip and fluence

- 239 - JAERI-Conf 99-009

120 I 110 5 100

2 90 o fc 80 O Segment B D Segment C 1 70 < .S 60 o S '

a 0.8 1.0 1.2

Neutron Fluence (x 10"n/mJ, E > lMeV) Fig. 5 Relationship between change in absorber outer diameter and neutron fluence

i 10.2 r

1 10.1 - A = 1.8% ^<^^ bO 10.0 - HH Segment A 9.9 HH Segment B Q Segment C

9.8 1 1 >j • 0 100 200 1826 Distance from Control Rod Tip (mm)

Fig.6 Density deviation of absorber tips

•e- "X.

10mm 58mm

Thickness: About 0.5 mm

Fig. 7 Tensile test specimen taken from segments A, B and C

- 240 - JAERI-Conf 99-009

Axial Crack

'Outer Surface

Inner Surface

5mm (a) Low Magnification 100 fim (b) High Magnification

Fig. 8 Typical metallography of the cladding crack in segment B (114mm above rodlet tip)

1 7 inner forced fracture surface surface

\ \ crack surface crack front outer surface

1mm

Fig.9 Crack Surface of Rodlet Cladding Tube

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crack front forced fracttxre region outer surface

inner surface

100 IJ in

Fig. 10 SEM investigation of the fracture surface of rodlet No.l

0.1mm

50 10

6 Fig.l 1 SEM investigation of the fracture surface of the tencile test specimen(Segment B,320°CN 6 X 10" /s) - 242 - JAERI-Conf 99-009

A BWR A 0 BWR D 200 O BWR B a BWR E Ref.(7) 0 BWR C • PWR

160

l i i 100 i

|H-O37« tOG Ref .(7)

60

10 10 10 10 10 10 10 1 nuance (F) n/m (E > lMeV) v

Fig.12 Hydrogen content of irradiated Type 304 SS as a function of fast neutron fluence

initiation limit

Elapsed time Elapsed time

(1) IAMC (2) IASCC

Fig.13 Comparison between IAMC and IASCC

- 243 - Neutron Fluence at Rodlet Tip (xlOVcm2, E > lMeV)

0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8

150 Estimated Maximum Increase in Outer Diameter of Conventional RCCA

0.7%

0) Critical Diameter 50 Increase .Estimated Maximum > Increase in Outer a I Diameter for Increased to Gap 5 •po CD n o 6 O Q 0 VO

-50 Critical Fluence for Critical Fluence for Conventional RCCA (~3 x 10°) Increased Gap 8

-100 I : 0 2 3 4 5 6 Neutron Fluence at Rodlet Tip (x lO^n/cm2, E>0.625eV)

Fig. 14 Illustration showing the concept of the countermeasures. JP9950644 JAERI-Conf 99-009

3.3 Surveillance Tests for Light-Water Cooled Nuclear Power Reactor Vessels in IMEF

Yong-Sun CHOO, Sang-Bok AHN, Dae-Gyu PARK, Yang-Hong JUNG, Byung-Ok YOO, Wan-Ho OH, Seung-Je BAIK, Dae-Seo KOO and Key-Soon LEE

Korea Atomic Energy Research Institute, Irradiated Materials Examination Facility P. O. Box 105, Yusong, Korea, 305-600

ABSTRACT

The surveillance tests for light-water cooled nuclear power reactor vessels were established to monitor the radiation-induced changes in the mechanical properties of ferritic materials in the beltline according to US NRC 10 CFR 50 App. G, US NRC RG1.99-rev.2, ASTM E185-82 and E185-94 in Irradiated Materials Examination Facility(IMEF). The surveillance capsule was transported from NPPs pool sites to KAERI IMEF by using a shipping cask. The capsule was cut and dismantled by capsule cutting machine and milling machine in M2 hot cell. Charpy tests and tension tests were performed in M5a and M5b hot cells respectively. Especially the EPMA located at hot lab was used to analyze the Ni and Cu wt% composition of base metal and weld for predicting the adjusted reference temperature(ART). The established process and test results were summarized in this paper.

I. INTRODUCTION

The mechanical properties of ferritic materials in the beltline of light-water cooled nuclear power reactor vessels should be periodically tested and monitored, so called surveillance tests, to investigate the radiation-induced changes according to US NRC 10 CFR 50 App. G, US NRC RG1.99-rev.2, ASTM E185-82 and E185-94[l,2,3]. The surveillance tests in IMEF were established at the end of 1994 and have been continuously performing since the middle of 1995. The surveillance test processes, such as transportation of irradiated capsule from NPPs pool sites to KAERI IMEF, cut and dismantling of the capsule, Charpy tests, tension tests, and analysis of chemical composition for base metal and weld metal, were successfully accomplished . The flow diagram of

- 245 - JAERI-Conf 99-009 surveillance tests is described in Fig. 1. In this paper the established process and the typical test results were summarized.

II. EXPERIMENT

1. Transportation The surveillance capsule was transported from NPPs pool sites to KAERIIMEF by using a 2.5 ton shipping cask and a 5ton truck. At cask receiving area of IMEF the shipping cask was unloaded by the 30ton fixed hoist and loaded to the 30ton transfer cart to move to intervention area. After unbolting the bolts of outer shipping cask, the inner shipping cask was lifted out horizontally and set upright to move into the pool by 30/5ton overhead crane. As the shipping cask was carefully put on the bottom of pool, the shipping cask cover was opened by special tool and the irradiated capsule was taken out of the cask. The capsule was moved to the basket of the bucket elevator, installed in the pool, and elevated into Ml hot cell. In Ml hot cell the capsule was lifted by the l.Oton in-cell crane and Model E-HDE master-slave manipulators shown in Fig. 2 and transferred to M2 hot cell to cut and dismantle.

2. Cut and dismantling^] The dimension of capsule is 1.182"xl.0"x56" and the shape is shown in Fig. 3. The material of capsule is stainless steel and the top circular bar and the bottom square bar of capsule were welded to the front and back plates of capsule each other. The top and the bottom parts of capsule were cut thoroughly by capsule cutting machine, as shown in Fig. 4, specially designed for cut the HANARO fuel assembly and capsule irradiated in HANARO. The revolution of wheel and the feeding speed was 300rpm and l.Omm/min. respectively. It took 27 and 28minutes to cut completely top and bottom parts of capsule. After cut them, the burr was not found at the cut surface at all. The milling machine was used to cut the front and the back sealed welding lines as shown in Fig. 5. It has a little difficult to cut the welding seam line at once without resetting the capsule on the bed of milling machine because the capsule length is longer than the bed. It took 4hours to only cut the front and the back welding seam lines on cutting condition that x-motion's speed is about 6mm/min. and the revolution of bite is 300rpm. After finishing cut of the front and the back plates of capsule, the capsule was dismantled to pull the front plate toward upward using master-slave manipulators. The location of specimens, thermal monitors, and dosimeters was exactly accorded with capsule diagram and

- 246 JAERI-Conf 99-009 fabrication drawing. The number of Cv specimens, tension specimens, CT specimens, bend specimen, dosimeter block, and shim blocks which contain dosimeters and thermal monitor is 60, 9, 12, 1, 1, and 3, respectively. To take out the steel wire of dosimeter and thermal monitor from shim block, the bottom and the top of that were cut by micro cutting machine installed in M3 hot cell. Each shim block has five(5) dosimeters and one(l) thermal monitor. After cutting and dismantling the shim block, the small and transparent plastic bottles were used to store and to keep information of location for dosimeters. The plastic bottles contained dosimeters were transferred to glove box installed in the intervention area. All dosimeters were took out out of the plastic bottle in the bath on the table and classified. Especially one of them, which is used for measuring the fast neutron, was disassembled by cut the Cd cover. The dosimeter block, contained U238 and Np capsules, was also processed by milling machine to cut about 8mm from welded top face of dosimeter block and took out two capsules from holes and also get those into two plastic bottles.

3. Storage and distribution All dismantled and classified specimens including dosimeters and thermal monitors were moved to M4 hot cell. Sixty(60) Charpy impact specimens were distributed to M5a and nine(9) tension specimens were distributed to M5b hot cell. The dismantled steel wires are moved to chemical analysis department to analyze the neutron fluence. The others are stored in M4 hot cell.

4. Charpy tests[5,6,l] The model of impact tester is Tinius-Olsen model 84 equipped the instrumented tup and the capacity is 41.5kg-m(= 406J). The test temperature of specimen can be controlled by heating and cooling furnace from -150 to +300°C. The temperature of specimen is measured by thermocouple with accuracy ±1°C. Before breaking the specimen at the anvil by hammer the specimen heat or cool 30minutes and hold 30minutes to maintain temperature equilibrium. To measure the lateral expansion, the dial gage was used. All of apparatus concerned with surveillance were certified by National Standards Research Laboratory. The irradiation exposure set per capsule consists of base, reference, weld and weld heat affected zone(HAZ) and each material has 15 specimens respectively. According to ASTM El85-94 at least twelve(12) specimens are conducted to establish a full ductile-brittle transition temperature(DBTT) curve of material. All tested specimens were stricken within 5 seconds successfully. For each test specimen, absorbed energy, lateral expansion, and percent shear fracture

- 247 - JAERI-Conf 99-009

appearance were measured with using the digital display, dial gage, and CCTV, respectively. The DBTT curves for each material were described by using the regression method. The typical test results and fracture surfaces of specimens are shown in figure 6 and 7, respectively.

5. Tension tests[S,9,\0] The model of tension tester is Instron model 8502 and the capacity is lOton. The test temperature of specimen can be controlled by heating and cooling furnace from -150 to +300°C and the temperature of specimen is measured by thermocouple with accuracy ±1°C. The specimens were tested after heating and/or cooling the specimen 30 minutes and holding 30 minutes to maintain temperature equilibrium. The irradiation exposure set per capsule consists of six (6) base and three (3) weld metal. The test temperature of base, reference and weld was 68°F, 547°F, respectively. For each test specimen, the yield strength, tensile strength, fracture load, fracture strength, fracture stress, total and uniform elongation and reduction of area were measured and determined by using the CCTV and sealer. The typical test results are shown in figure 8.

6. Chemical composition analysis The Ni and Cu components should be analyzed, according to U.S NRC RG1.99-rev.2, to consider the chemistry factor comparing the analyzed data between before irradiation and after irradiation of base and weld metal. To analyze the change of Ni and Cu wt%, the sample preparation of cutting, mounting, grinding and polishing was done in M3 hot cell. The EPMA, which is manufactured by CAMECA in France, was used for analysis of C, Mn, Mo, Cr, Al, Co, etc.. The standard specimens were applied before scanning the specimen surface to minimize the error and to ensure the result with accelerating voltage and current intensity 15.0kV, 30nA, respectively. About 30 points were scanned by beam size lj^n along the 200#m distance. The typical analyzed data are plotted as shown in Fig. 9.

7. Evaluation of radiation induced changes The adjusted reference temperature(ART) of base and weld metal was evaluated to

combine the initial nil-ductility reference temperature(RTNDT), the transition temperature shift( ARTNDT), and margin.

- 248 - JAERI-Conf 99-009

III. CONCLUSIONS

The surveillance test processes, including the evaluation of radiation induced changes, such as transportation of irradiated capsule from NPPs pool sites to KAERI IMEF, cut and dismantling the capsule, Charpy tests, tension tests, and analysis of chemical composition for base metal and weld metal, were successfully accomplished. The test results were also fully satisfied the requirements of US NRC 10 CFR 50 App. G, US NRC RG1.99-rev.2, ASTM El85-82 and El85-94.

REFERENCES

1. Code of Federal Regulations, 10 CFR Part 50, Appendix G, "Fracture Toughness Requirements", Federal Register Vol. 60 No. 243, December 19, 1995. 2. Regulatory Guide 1.99, Revision 2, "Radiation Embrittlement of Reactor Vessel Materials", U.S Nuclear Regulator Commission, May 1998. 3. ASTM El85-82, "Standard Practice for Conducting Surveillance Tests for Light-Water Cooled Nuclear Power Reactor Vessels", E7O6(1F), in ASTM Standards, Section 3, American Society for Testing and Materials, Philadelphia, PA, 1993. 4. Y.S Choo, D.G, Park, S.B Ahn, B.O Yoo, and W.H Oh, "The Development of dismantling Machine for Capsule and HANARO fuel bundle irradiated at HANARO", KAERI/TR- 1078/98, KAERI, 1998. 5. ASTM E23-93a, "Standard Test Methods for Notched Bar Impact Testing of Metallic Materials", in ASTM Standards, Section 3, American Society for Testing and Materials, Philadelphia, PA, 1993. 6. Y.S Choo, K.S Lee, K.P Hong, D.G, Park and S.B Ahn, "Surveillance test(impact test Examination Technique Development in Hot-cell", KAERLTR-945/98, KAERI, 1998. 7. K.P Hong, Y.S Choo, S.B Ahn, Y.H Jung, and K.J Park, "Study on the Behavior of Irradiated Materials during Long Term Storage/Development of Irradiated Material Examination Techniques", KAERI-NEMAC/RR-107/93, KAERI, 1993. 8. ASTM A370-92, "Standards Test Methods and Definitions for Mechanical Testing of Steel Products", in ASTM Standards, Section 3, American Society for Testing and Materials, Philadelphia, PA, 1993. 9. S.B Ahn, K.S Lee, D.G Park, K.P Hong, and Y.S Choo, "The Improvement of Dynamic Universal Testing Machine for Hot Cell Usages", KAERFTR-1089/98, KAERI, 1998. 10. S.B Ahn, K.P Hong, D.G Park, Y.S Choo, and B.C Kim, "The Development on Tensile

- 249 - JAERI-Conf 99-009

Test Technique in Reactor Surveillance Specimens", KAERLTR-1087/98, KAERI, 1998.

TOANSPOTATION FROM NPPs POOL TO IMEF

UNLOADING at C@sk deceiving Area

MOVE into INTERVENTION AREA i ,

I,

PUT the SHIPPING CASK into POOL

CAPSULE WITHDRAWL

MOVE CAPSULE FROM POOL TO MI HOT CELL

CUTTING AND DISMANTLING IN M2 HOT CELL

SPECIMENS WITHDRAWAL AND CLASSIFICATION

TESTS OF ..«.'/. IMPACT TEST, TENSION TEST, AND CHEMICAL ANLYSIS

RADWASTE TREATMENT (IMEF -» Monolith)

Fig. 1. Flow diagram of surveillance test.

- 250 JAERI-Conf 99-009

Fig. 2. Photography of capsule movement from pool to Ml hot cell.

IRRADIATION

Houainu IRRADIATION CAPSULEUNYERNALS) Fig. 3. Schematic capsule diagram showing location of specimens, thermal monitors and dosimeter materials.

- 251 - JAERI-Conf 99-009

Fig. 4. Photography of capsule bottom cutting by capsule cutting machine in M2 hot cell.

Fig. 5. Photography of the front welding seam line of capsule cutting by milling machine in M2 hot cell.

- 252 - JAERI-Conf 99-009

200 i 1 1 1 1 1 1 ! 1 Base Metal (ST)

-

150 -

.-*•'*•' • =3 V • f T CD _ c 100 - 111 >' ^ " ' '*•' "" / l O ' m - • < 50 - unirradiated j v/ o firs! | / ,1 second | V third f w 0 .,,,,1,,,,(„ ,1 1, I i. 1 J f 1 I 1, !„ 1 i i 1 ,,„! In *,„ ,f ,,„! t ,) &,„.,* , -200 200 400 600 Temperature ( ° F)

Fig. 6. Typical Ductile-Brittle Transition Temperature Curve of base metal.

,1 1.'•:''.* 4-v!-

BG38

•Sj 5»Vi'^

?

MM9

%^H '''SI1

Fig. 7. Typical Charpy impact specimen fracture surfaces.

- 253 JAERI-Conf 99-009

120 1 i • i i

Base Metal (ST) •

100 - •—. ~~~~ * -__ • a-.. ULTIMATE TENSILE STRENGTH 0 fl---- 80 - - ^—^

&-• A-. . A 60 - 0.2% YIELD STRENGTH

40 -

20 - - Open : unlrradlated Closed : third

i . i . t i I 100 200 300 400 500 600 Temperature ( ° F)

Fig. 8. Typical tensile properties of base metal.

1000

100

0.01

1E-3 20 30 40 point no.

Fig. 9. Typical result of chemical composition analysis by EPMA.

- 254 - JAERI-Conf 99-009 JP9950645

3.4 The Fracture Toughness Testing of Unirradiated and Irradiated

Zr-2.5Nb CANDU Pressure Tube

Sangbok AHN°, Dosik KIM0, Daeseo KOO", Sangchul KW0N2), Yongsuk KM2) Korea Atomic Energy Research Institute P.O. Box-105, Yusong, Daejon, Korea

ABSTRACT

The test techniques of fracture toughness test for irradiated Zr-2.5Nb CANDU pressure tube materials were developed in hot cell. The curved compact specimens of 17mm in width with a notch in the axial direction were made directly in the hot cell from the irradiated and unirradiated Zr-2.5Nb pressure tubes using a specially designed electric discharge machine (EDM). The crack growth was measured by reversing direct current potential drop method. J- Integral was determined from the measured load and displacement value accordance with ASTM E813, E1152 and 1737. The tests of the unirradiated and irradiated Zr-2.5Nb specimen with fluence 8.9xl022n/m22 were conducted in hot cell. The dJ/da of the unirradiated Zr-2.5Nb pressure tubes agreed well the measured values on the same tubes out of hot cell. The toughness of the irradiated specimen was dropped drastically comparing to the unirradiated. Further, the fractographies of the irradiated Zr-2.5Nb pressure tubes were discussed to investigate the neutron effect on the fracture toughness of Zr-2.5Nb pressure tubes.

INTRODUCTION

Since the Wolsung Unit 1 has started operation in 1983, 3 PHWRs (Pressurized Heavy Water Reactors) currently are in operation and one more will start operation in the late half of 1) Irradiated Material Experimental Facility 2) Zirconium Development Team

- 255 - JAERI-Conf 99-009

1999. Thin-walled pressure tubes of cold worked Zr-2.5Nb (nominally 6.3m long, 103mm in diameter, and 4.2mm thick) is used as the primary containment for the uranium dioxide fuel. Heavy water flows through the tubes to cool the fuel, under an internal pressure of about 10 MPa and at a temperature range from about 260 to 320 °C. Over the expected lifetime, the pressure tube is subjected to degradation due to exposure to high stresses, temperature and neutron flux. One criterion for lifetime of a tube would be an inability to defend leak-before-break (LBB). This condition can be met if LBB if a crack initiate, penetrates the tube wall and leakage of heavy water is detected before the crack grows the critical crack length(CCL) and become unstable. The critical crack length is governed by fracture toughness [1]. Thus, it is necessary to characterize the fracture toughness of the Zr- 2.5Nb pressure tubes with neutron irradiation till the lifetime of 3x1026 n/m2. In the fast, fracture toughness was characterized by slit burst tests which were very expensive, consumed a lot of material, and could not be used on a burst tube.[2-4] Therefore, it was desirable to develop small specimen test methods in hot cell. The objective of this study is to evaluate the feasibility of a fracture testing procedure for irradiated Zr-2.5Nb pressure tubes. By using the curved compact tension specimens cut away from Zr-2.5Nb pressure tubes by a specially designed electric discharge machine, crack growth resistance of unirradiated and irradiated Zr-2.5Nb pressure tubes was determined. Their dJ/da values obtained in the hot cell were compared with the reported values or the measured values out of the hot cell to identify the feasibility of the fractue toughness testing procedure. The middle ring of Zr-2.5Nb pressure tubes were used in this study, which had been operated in Wolsung Unit 1 for 10 years with the neutron fluence of 8.1x1025 n/m2.

DEVELOPMENT OF EXPERIMENTAL PROCEDURES IN HOT CELL

1.Material andspecimen preparation. Non-irradiated and irradiated Zr-2.5Nb pressure tube materials were used in this study. The tube are manufactured by extrusion, after p-quenching, of hollow forged billets at a temperature of about 815-850°C, i.e., in the (a+p)-phase field. The Specimen was cut from tube with retaining original curvature by EDM in hot cell. The

- 256 - JAERI-Conf 99-009 cutting condition was 6-8Ampere in currents and 0.2jisec in on time. The inplane dimensions were in the ratio to specimen width, w, as described in ASTM E 813, and the thickness and curvature were identical to those of tube. The detailed dimensions of the 17mm curved compact tension(CT) are as Figure 1. A simple analytical calculation estimates that the maximum curvature-induced stress was less than 10% of the inplane tensile stress at the crack tip[5]. By comparing results from the flat and curved specimens, the equation of flat- plate J-integral can be applied to both specimen types to calculate the fracture toughness parameters with little error.

2. Equipment Apparatus For the test the Instron 8502 machine with furnace and 1 ton load cell was used. The test fixture consisted of pull rods and grips to be electrically insulated from the test machine to prevent short circuiting from DCPD currents. The insulated grip shape is in Photo 1. The pins were made from hardened steel to minimize pin deflection and had tapered to 1.5° for producing straighter fatigue precrack in Figure 2. These pins distribute more loads to the outside surface of the specimen to compensate for the bending stress caused by the curvature of the specimen. To measure load-point displacement, an alternate method to measure the movement of grips was adopted with LVDT pick up device in Photo 2. The displacements were corrected with values obtained from the measurement of deflection in a rigid specimen, over the full load ranges. The measurement method of crack extension was by the reversing DCPD described in reference. [6] The power supply lines were attached to the upper and lower sides using brass cap. The lead wires to measure dropped voltages were dia. 0.6mm Nickel-Copper electric lines and were attached to the crack mouth of the specimen by spot welder. The welding condition was 3000A in current and 0.2sec in pressuring time.

ITestPnxedures The specimen was carefully inserted in the grips and connected with pins so as not to disturb the potential leads. The DCPD system were switched on and allowed to be stabilized until the potential drop indicated that there were no more voltage changes for at least 20 min. The fatigue precracking was carried out in the spirit of ASTM E 399 section A22. To initiate the fatigue crack evenly, an initial stress intensity factor range (AK) about 15 MPaVm.

257 - JAERI-Conf 99-009 with the load ratio(R) of 0.2. Once the fatigue crack was started, AK was decreased. The loading cycles were 5Hz. The AK used for the last 0.5mm of fatigue crack was on the order of 11 MPaVm. The final fatigue crack length was enough to have an a/w value of about 0.5. To the end of fatigue, the crack growth is monitored by the potential drop signal using an estimated value from the unirradiated specimen calibration constant. The J-integral test was carried between 2.5-4 mm of crack extension. The displacement increasing speed is 0.25mm/min. Throughout the test, the values of load, load point displacement, dropped voltage and specimen temperature were to be continuously monitored. The sampling rate for the data acquisition system was 150 points for each unloading procedure. At the end of test the final crack length was marked by heat tinting for 20 min. at 280~290°C. During the tinting procedure a small load (approximately 50% of the final load) was applied to the specimen to prevent crack closure. The initial and final crack lengths were measured by the nine point average method with highscope system. From the total dropped voltages and crack growth, the calibration constant was derived to calculate the crack increments during the test. Using the data from the test, the J-integral was calculated according to ASTM E-1737 to generate the J-resistance(J-R) curve. The J value was calculated from the next equations.

J,=J*+J* (1)

Where JeI and JpI are the elastic and plastic component of J-integral, respectively

2 2 Jd=K, (l-v )/E (2) Where B is the specimen thickness, v is the Poisson's ratio, E is the Young's modulus and;

0.886 + 4.64(a,. / w)- 13.32(a, / w) f(at/w)=- (3) •14.72(fl,./w)3-5.6(a,./w)4

The value of Jpl was calculated using the equation derived by Ernst et al.[7] and Clark and Landes[8]

J •'/>'(<) "~ (4)

Where b is the ligament (w-a^, T], = 2.0+0.552(b/w) and y{ = 1.0+0.76(b/w). The value of

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Apl(i)- ApKJ.,) is the increment of plastic area under the load and load point displacement record between lines of constant displacement at point (i) and (i-1)

A p AP«» = P,O-» + i( i + Pi-i X<5 pun - * P((M>) / 2] (5)

Where 5pli is the plastic part of the total load line displacement, 8.

tpm^ti-PiC, (6) Where Ci is the specimen compliance and given by

2 3 • 12.219(a; / w) - 20.065(a,. Iw) - 0.9925^ / w) ' 4 5 (6) E*B [ w - at + 20.069(a,. / w) - 99314(9.9314(aa , / w) Where E* (=E/(l-v)) is the effective Young's modulus.

RESULTS AND DISCUSSION

Figure 3a, b show load vs. displacement curves with the ratio(a/w) of about 0.53 for the unirradiated and irradiated Zr-2.5Nb tubes at room temperature. The unirradiated Zr-2.5Nb tube had a continuous change in load and voltage with displacement. In contrast, the irradiated tube had a discontinuous increment in load and voltage with displacement due to a series of crack jump occurring during fracture at room temperature. It is worth noting that the irradiated Zr-2.5Nb tube has the lower maximum load and earlier crack initiation than the unirradiated Zr-2.5Nb tube. It was reported that the lower temperature, the longer jump[9]. Quantitative evaluation of the embrittlement of Zr-2.Nb pressure tube by neutron irradiation can be made by plotting J-R curves of pressure tubes. First, the crack distance of the unirradiated and irradiated Zr-2.5Nb specimen was determined by using the 9 point method on the fractured surfaces shown in Photo 3a, b. Through the measured crack distance and J- integral calculated from the load-displacement curve, the J-R curves were plotted for the unirradiated and irradiated Zr-2.5Nb as shown in Figure 4a, b. The J-R curve for the unirradiated Zr-2.5Nb had a continuously decreasing slope. However, the J-R curve for the irradiated one consists of three stages; the stage I where the crack starts to propagate followed by a decreasing slope of the J-R curve, the stage II where the slope of the resistance curve steeply increases, and finally the stage lU where the slope decrease and approaches a

- 259 - JAERI-Conf 99-009 constant value. The results shown in Figure 4b confirm that the irradiated Zr-2.5Nb has much decreased low fracture toughness compared with that of the unirradiated one. From the J-R curves, we determined the dJ/da as a fracture toughness value, the linear slope of the J-R curve between the 0.15 mm and 1.5 mm exclusion lines as defined by ASTM E 1152 and E

1737. It is because the crack initiation value, JIC defined in ASTM E813 standard could not be reproduced consistently on this curved compact tension Zr-2.5Nb specimen due to the geometric limitation [10]. Table 1 shows the measured dJ/da values for the unirradiated and irradiated Zr-2.5Nb tubes.

Table 1. Fracture toughness results for the Zr-2.5Nb materials from CANDU pressure tube.

dJ/da J-Integral Value Specimen Test (MPa) (kJ/m2) Identity Temp. Meas Ref. 0.2mm 1.5m Max load Reference (°C) m UR-01 25 329.7 155.8 575.7 221.6 Unirradiated UR-02 25 339.5 342.1° 165.5 580.5 230.0 Unirradiated IR-01 25 84.5 33.7 134.2 99.12 Irradiated IR-02 25 58.5 25.92) 22.5 102.3 73.5 Irradiated

+ 1) tested out of hot cell 2) tested at AECL The measured dJ/da values of the unirradiated Zr-2.5Nb pressure tube in the hot cell were quite in good agreement with those conducted on the similar specimen out of the hot cell. However, the determined dJ/da values at room temperature for the two curved compact tension specimens were found two times as much as dJ/da values reported by Han[l 1]. The uncertainty of dJ/da values for the irradiated Zr-2.5Nb pressure tubes is under scrutiny. Photo 3-a,b show the fractographs of curved compact specimen from unirradiated Zr-2.5Nb pressure tube. The unirradiated ductile specimen had the crack with a thumbnail shape which is quite symmetric with respect to the thickness of the compact tension specimen. The material removal sometimes was observed in the middle of the fractured surface even though its cause is yet to be investigated. Photo 4-a,b,c,d,e shows the SEM microstructures taken from various parts of the fractured surface of the unirradiated Zr-2.5Nb tube. The fractured surface just in front of the fatigue shows very fine dimples along with little fissures (Photo 4-

- 260- JAERI-Conf 99-009 a). However, at the middle of the fractured surface, some fissures appeared along with some small voids (Photo 4-b and c). Some clear fissures, however, appeared just before the ductile shear region (Photo 4-d). One thing to note is a considerable through-thickness yielding for this unirradiated specimen with very narrow shear lips near the surface (Photo 4-e). In contrast, the irradiated Zr-2.5Nb specimen had little through-thickness yielding and, furthermore, well-developed flat fractured surface along with a slant fracture developing at the surface as shown in Photo 5-a and b. Some long fissures, lying in the tube axial direction, were observed in the middle section of the flat fractured surface as shown in Photo 5-c. However, fissure density looks quite low in comparison to that on Zr-2.5Nb pressure tubes of low fracture toughness [5], implying that the irradiated Zr-2.5Nb tubes under investigation seem to be of high toughness. On the other hand, near the end of the flat fracture region, the fracture proceeded at 45 degrees to the transverse-axial plane which seems to correspond with the plane of the maximum shear stress. There was no evidence of fissure formation but of equiaxed and tearing dimples near that region as shown in Photo 5-d. These results lead to a conclusion that neutron irradiation embrittles Zr-2.5Nb pressure tubes qualitatively

CONCLUSION

The test technique for fracture toughness was developed for the curved 17mm CT specimen from CANDU pressure tube in hot cell. The specimen was cut by EDM retaining original tube shape. The crack increments were measured by DCPD system. The data from test were analyzed based on ASTM E813, El 152 and E1737. The conclusions we have drawn from this study are summarized as in the following:

1. J-R curves of irradiated and unirradiated Zr-2.5Nb pressure tubes were successfully measuured in the hot cell by using the curved compact tension specimens. The irradiated Zr-2.5Nb pressure tubes had lower dJ/da values than that of the unirradiated Zr-2.5Nb. The dJ/da of the unirradiated Zr-2.5Nb pressure tubes agrees well with the measured values on the same tubes out of the hot cell. However, compared to the reported values of the similar irradiated Zr-2.5Nb pressure tubes, the measured dJ/da values of the irradiated Zr-

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2.5Nb pressure tubes were found higher, the cause of which has to be elucidated further.

2. The fractured surface of irradiated Zr-2.5Nb pressure tubes consists of flat fracture region and slant fracure developing at the surface while the unirradiated Zr-2.5Nb pressure tubes had considerable through-wall thickness yielding.

REFERENCES

1. Hosbons, R. R., Davies, P. H., Griffiths, M., Sagat, S. and Colmann, C. E.: ASTM 12th Symposium on Zirconium in the Nuclear Industry Abstract Paper, 1998 2. Langford, W. J. and Mooder, L.E.J., International Journal of Pressure Vessels and Piping, Vol. 6, 1978,pp275-310. 3. Cowan, A. and Langford, W. J., Journal of Nuclear Materials, Vol.30, 1969, pp. 271- 281.Wilkins, B. J. S., Barrie, J. R, and Zink, R. J., Report AECL-6195, AECL, 1978 4. Wilkins, B. J. S., Barrie, J. N., and Zink, R. J., Report AECL-6195, AECL, 1978 5. Chow, C. K. and Simpson, Leonard A., Fracture Mechanics: Eight Symposim, ASTM STP 945, 1988, pp. 419-439 6. Dosik, KIM et al. KAERI-JAERI Joint Seminar, 1999. 7. Ernst, H. A., Paris, P. C. and Landes, J. D., Fracture Mechanics: Thirteenth Conference, ASTM STP 743, 1981, pp. 476-502 8. Clark, G A. and Landes, J. D., Journal of Testing and Evaluation, vol.7, No.5, 1979, pp. 643-662 9. Chow, C. K., Colman, C. E., Hosbons, R. R., Davies, P. H., Griffiths, M., and Choubey, R., ASTM STP 1132, 1991, pp. 246-275. 10. Candu Owner Group, Instructions to Round Robin Participants, COG-98-161-1, RC-2069 1,1998, pp 21-28. 11. Private Communication with B. S. Han, KEPCO

- 262 - JAERI-Conf 99-009

•I

Figure 1. Dimensions in 17mm compact tension specimen

Figure 2. Tapered loading pin for precrcking

"-1

A- "i . r

Photo 1. Electric shielding device for DCPD System Photo 2. LVDT pick up device

- 263 JAERI-Conf 99-009

1 2 Displacement [mm]

Figure 3-a. Typical load displacement curves Figure 3-b. Typical load displacement curves for the unirradiated specimen for the irradiated specimen

Corulniction Una 1000 (MSmm Comtructton o.15mm ;' Jr Exdmion Unt Un* Exdmkn Urw • mir /j I / •'/ • / .'•• • S" 500 / •'••' •

/ •'• * // :7•'•: " • U^_i5mm /r• ji 0.2mm £ jl*- OHs* lint

1 2 3 Crack Increment, 4a[mm] Crack Increment, Aa [mm] Figure 4-a. Typical J-R curve Figure 4-b. Typical J-R curvee for the unirradiated specimen for the irradiated specimen

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t

Photo 3-a. The Facture surface Photo 3-b. The fracture surface of the unirradiated specimen of the irradiated specimen

(Photo 4-a)

(Photo 4-b) (Photo 4-c)

'ij vyif''" i (Photo 4-d) (Photo 4-e) Photo 4. SEM images from the unirradiated Zr-2.5Nb fractured surface

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I V

(Photo 3 a) (Photo 5-b)

(Photo 5-c) (Photo 5-d) Photo 5. SEM images from the irradiated Zr-2.5Nb fractured surface

- 266 - JP9950646

3.5 POST-IRRADIATION EXAMINATION OF PWR FUELS IN KOREA

Yong-Bum Chun, Gil-Sung You, Dae-Seo Koo Eun-Ka Kim, Duck-Kee Min, Seung-Gy Ro

PIEF, Nuclear Fuel Cycle Examination Team Korea Atomic Energy Research Institute 150, Dukjin-dong, Yusong-ku, Taejon, Korea

ABSTRACT

Post-irradiation examination of reactor fuels relevant to the failure mechanism were conducted. Several fuel assemblies identified to have been damaged during power operation were transferred to PIEF to search for the causes of failures. The apparent geometrical changes and deformation of the fuels were inspected and the subsequent precise hot cell examinations were followed. In this paper, concentrations were put on to the PIE especially for the defective fuels irradiated at NPPs in Korea.

INTRODUCTION

Two fuel assemblies irradiated at NPP were identified as failed through inspection. Each fuel assembly had one failed rod. Both fuel assemblies were determined to be repaired for continued operation in the reactor. Visual inspections were performed on the failed rods and the fuel assemblies in order to determine the causes of failure. Based on the preliminary analysis of the inspection data, it is postulated that the failure mode for one rod (K-rod) is due to an internal mechanism. However, the actual root cause is indeterminate from the inspection performed. The failure mode for the other fuel rod (R-rod) is a small through-wall hole, most likely caused by a sharp piece of debris that became entrapped within the grid cell occupied by this rod. The failed fuel rods were extracted and transferred to PIE facility for more precise hot cell examination.

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Visual inspection of K-rod indicated the presence of several regions of secondary hydride damage, but no indication of the location of the primary defect site. Ghost (white-colored) hydride regions were observed at 1,592 mm and 1,420 mm below Zircaloy- 4 Grid #4. An open blister region was observed at 1,177 mm below Grid #3, with some material missing from a single fuel pellet visible at this location (Fig. 1, 2 and 3). A brittle region extended about 7.2 rnm above the blister. Axial cracks were observed in this region, and some surface oxide and crud appears to be removed. An axial crack was also observed within the ghost hydride region at 1,592 mm. The visual inspection did not reveal any indications of fretting wear along the rod that could have been .caused by either debris or grid- to-rod contact. Nor was there any visual evidence of, or reason to believe that any other external failure mechanism or operational Fig.l.K-rod at 1,420 mm condition may have been involved. For example, excessive waterside corrosion or pellet-cladding inter- action (PCI) could not be involved, since the assembly bum-up was very low at the time of failure. Since the visual inspection of K-rod did not indicate any potential external causes, it is postulated that the failure cause is due to an internal mechanism. However, the actual root cause is indeterminate from the inspection performed. Internal Fig.2.K-rod at 1,592 mm Fig.3 .K-rod at 1,177 mm failure causes found in Zircaloy-clad fuel over the past several decades are generally associated with fabrication processes and have included such as; 3 primary hydriding that may be caused by a high moisture content of fuel pellets, water remaining in tubes before welding, of the presence of other material contaminations within the fuel rod following fabrication that might be a source of hydrogen. S inter-connected porosity in end-cap material S end-cap weld defects that cannot be identified during a single rod visual examination.

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Visual inspection of R-rod L'J' 9C" indicated the presence of a small through-wall hole at approximately 93mm from rod bottom (Fig.4), which is located within the upper half of the bottom Inconel spacer grid. There is no evidence of any grid-to- rod fretting wear in this region. The through-wall hole, therefore, was most likely caused by a sharp Fig.4. R-rod Image around 93 mm piece of debris that became entrapped within the grid cell occupied by R-rod. This small through-wall site is believed to be the primary defect site. Additional areas of damage on the rod caused by secondary hydride failure were observed at 2,660 mm with a long axial crack below Zircaloy-4 Grid #7 and ghost hydride through Grid #7 region (Fig. 5). Since the probable piece of debris was located within the grid cell, and not below the grid cell, a reasonable expectation existed that the Fig.5. R-rod image around 2,660 mm surrounding rods were not damaged. However, if a piece of debris extended below the grid, neighbor rods to the R-rod may have been damaged during operation, although not failed. So, the eight neighbor rods surrounding R-rod were inspected for damage indications and no indications of external wear were found. Inspection of the spent fuel pool rack locations in the vicinity of the fuel assembly inspection stand were also performed to find a piece of debris that may have dislodged from the bottom grid cell during the inspection and no debris was observed.

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Concludingly, R-rod has typical features of a debris failure followed by secondary internal hydriding at a location some distance from the failure hole. In case of this rod, the debris, a small wire-like piece of foreign material, likely came from the coolant and was trapped at a bottom grid spring to cladding contact point. The coolant velocity likely caused the trapped debris to vibrate giving repeated contact of the ends of the wire-like debris with two different closely-spaced points on the cladding. The combined ZrO2 film mechanical damage plus rapid corrosion under the damage point is called debris fretting. LWR fuel cladding can and does develop a through-wall hole by this mechanism. Secondary hydriding occurred far-distance from the primary cladding hole by the well- known mechanism of progressive reduction of the PH20/PH2 (Partial pressure of steam to partial pressure of hydrogen) ratio. The reaction

Zr + 2H2O = ZrO2 + 2H2 oxidizes the internal side of the cladding tube in the area closest to the in-leakage hole. This creates a surplus of hydrogen that can attack the cladding inner surface in areas away from the primary defect, where oxidation has not yet occurred (or is damaged and unable to repair),

and the PH20/PH2 ratio is reduced below a critical value. The reaction

H2 + Zr =ZrH2

is exothermic and very rapid. Spherical segments of ZrH2 called "sunburst" or "Blisters" are formed, initially in compression. The blisters are brittle and crack due to power reduction (compressive stresses reverse). The high hydride concentration areas reveal themselves as cladding diameter bulges and cladding oxide gray blotchy areas. K-rod shows the most likely primary failure mechanisms which are (a) internal hydriding due to moisture trapped inside the sealed fuel rod during fabrication or (b) a very small fabrication defect in the end plug or in the weld at the bottom of the rod (the hydriding is at the higher part of the rod and must be far distant from the primary defect). These candidate mechanisms are those experienced historically that can and have occurred at low power and low service exposure. All other known failure mechanisms require higher burn-up or longer exposure time or high power, or a combination. Between the two candidate mechanisms, historically the internally trapped fabrication moisture is reported to have caused failures at least ten times more frequently. Failure mechanism of the longitudinal end plug solidification, "end plug piping" defect is very difficult to determine by inspection. Therefore, some believe the undetected occurrence of this type of failure may be as much as 10 times higher than reported.

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COOLANT RADIOACTIVITY DATA ANALYSIS

The plant fuel shows an abrupt increase in I131 release of about 1 -2xlO°V Ci/cc, at the end of July 1995 just after 50% of plant 100 power increment (Fig. 6). 0.1 7.31 Since the failed fuel rods I were both in the core 0.01 periphery, it is unlikely 1E 3 that one non-fuel- I " 40 Q. releasing failure could release this much. Thus 1E-4 nit 20 it is likely that the debris 8.17 failure occurred at that Jul21 Jul 31 Aug 10 Aug 20 Aug 30 Sep9 Sep19Sep29 time. This is supported Date by an observed Fig.6. Coolant Radioactivity in NPP continuing increase in the I131 activity. On August 16, a very large further increase is observed. The plant power decreased from 80% to 30%, and about 40 times of Iodine activity increase was detected. This indicates severe degradation, i.e., the observed axial crack occurred, or expanded, at that time. It is not possible to tell when the second failure occurred, since it is overwhelmed by the fuel-releasing one. After the severe degradation, the fuel release did not worsen too much. However, the level of activity did not decrease, which indicates that either the fuel release had stopped and all released fuel was firmly settled on fuel surfaces elsewhere in the core, or the fuel kept releasing enough to keep up with the coolant cleanup system, which is only capable of removing contamination dissolved and suspended in the coolant. It should be conservatively assumed that the Iodine, after the restart, and off gas activities will remain high, despite the removal of the failed fuel. The I131 level is 0.2 n Ci/cc which shows an abrupt increase at the end of July, i.e., at the suggested time of the first fuel release. The ratio of I131 to Xe133 shows an EOC value about 0.3, which is equal to its "tramp" value. This indicates that the activity release is dominated by released fuel (tramp). The ratio I134 to I131 shows a gradual decrease between the suggested first incident of fuel release and the severe degradation on August 15. This indicates a widening of the breach in the fuel-releasing rod. Concludingly, the root cause of the two failures is probably different for the two. One is a classic case of debris failure, the other either is internal hydriding of an unidentified external cause, possibly end cap "piping" or weld flaw. The coolant activity is much higher than the direct contribution from the failed rods. Significant fuel release from the rod failed by debris

- 271 - JAERI-Conf 99-009 fretting is suggested. The fuel release most likely began early, but was aggravated later (August 16):

EXAMINATIONS

Several fuel failure mechanisms were considered to find the root cause of failure. Concentrations on debris fretting, spacer grid fretting, primary hydriding, end-plug defect, and end-plug weld defect were put during the non-destructive and destructive examination. For R-rod, the cause of through-wall hole defect and the secondary hydride formation scheme were major concern. For K-rod, finding of other defect or failure except hydride failure and the hydride formation mechanism were major concerns of PIE.

R-ROD EXAMINATION

At first, for R-rod the orientation of fuel rod that was located in the assembly was determined and through-wall hole shape and dimension were inspected. Defect sizes measured were 0.9 mm and 0.3 mm in length and width, respectively. The defect locates at 93 mm from the bottom end of rod and was rotated about 70.3 ° from the front view. Eddy current test was conducted and no other noticeable defect signal was found except the Fig.7. ECT Result for R-rod defective zone(Fig.7). In X-ray radiography, no noticeable changes were detected and gamma spectroscopy result shows normal irradiation conditions (Fig. 8). And the vacuum leakage test for the end cap zone of the rod showed no leakage in both ends. In destructive test for R-rod, macro- and micro- structure of the pellet and cladding tube around defective area were examined precisely (Fig. 9 & 10). Inside and outside Fig.8. Gross Gamma Scanning Results of R-rod oxide layer thicknesses of the cladding tube

- 272 - JAERI-Conf 99-009 around through-wall hole area were measured. About 10 n m of oxide was measured around the grid spring contact area and 1 about 4 [im of oxide thickness was measured around the through- wall hole defect. The internal oxide thickness is about 4~5 times thicker than the external ones. While the external oxides layer distributions show almost uniform states with around 2 /J m of thickness, the internal oxides Fig.9. Thru-Hole Defect of R-rod Fig. 10. Thru-Hole Defect shows maximum 10.5 fim of measured value at 2,100 mm location (Fig. 11). The oxide thickness of internal clad shows a little bit higher values which means that the failure of this rod was made comparably —a—Internal Oxide earlier time of BOC. It is reported that the —e—External Oxide normal irradiated intact fuel used to show little oxide layers in internal clad surface. Fig. 12 shows a typical secondary hydride failure of R-rod located at 2,660 mm from the bottom end of rod. And the density of 500 1000 1500 2000 2600 3000 fuel pellet is 10.535-10.567 g/enf which shows very small discrepancies with the Fig.ll. Oxide-Layer Thickness of R-rod fabrication data of 10.55 g/cm3. It was expected from the bum-up measurement result of this rod and the measured bum-up was about 2,013 MWD/MTU. The macro- and micro-structure of R- rod showed similar structures to the un- j x irradiated UO2 structure except for the [ -> ,. - , ',?-,- - region between 1,300—2,120 mm where , '"'"*;

remarkable grain growth phenomena were Rg 12 Secondary Hydride Failure of R.rod shown. It is believed that the intrusion of coolant through the defect led to the oxidation of fuel pellet. Consequently, the O/U ratio increased which lowered the thermal conductivity of fuel and it finally contributed to the

raising of fuel temperature up to the temperature point enhancing the grain growth of UO2.

- 273 - JAERI-Conf 99-009

\ v! M A • B d

118-9 { A ) Fig.14. ECT Result for K-rod

{ H ) if..r, mi s.r-. ).iu Fig. 13. Macro- and micro-structure of Fuel Pellet of R-rodat2,100mm Fig. 15. ECT Result for K-rod

In K-rod, there are 4 suspicious regions showing extraordinary signals or results through NDT examinations. Cladding failures were observed around 1,177 mi and 1,592 mm region. Between two locations, ECT (Eddy Current Test) signal of a large defect was detected at 1,420 mm location, and finally internal flaw signal was detected at 276 im, but the magnitude was comparatively small (Fig. 14). X-ray radiography shows a normal stack states of fuel pellet. The gap interfaces between pellets were maintained in normal states. The average diameter of the fuel rod was 9.70±0.02 mm, and ovality conditions of the clad show normal states except the region around the hydride failure occurred. Gamma scanning examination was carried out to gather the irradiation information of fuel pellets by collecting the gross and specific gamma counts for several isotopes such as Cs, Nb and Zr (Fig. 15). In 30 minutes of leak test for the both end plug welds and end plug itself under the ixlO"3

274 - JAERI-Conf 99-009 torr. vacuum conditions, no noticeable leakage was detected. Because no other failure except the hydride blister failure was found in this rod, several postulations were set up and a series of examinations including the end plug metallographic examination was conducted according to the postulations. Fig. 16 shows the picture of fuel end plug section. A defect from surface to inner matrix

•/

o

:..'•

Fig.l6-a Fig.l6-b Fig.l6-c Fig.l6-d Fig. 16. End-plug Defect in K-rod material of clad can be identified. Small amount of resin intrusion is seen and about max. 30 //mof oxide layer formed around the defects can be seen. This failure might be connected to the internal plenum area of fuel rod but the defect size was too small to find the connection exactly. In fig. 16-d, the inner white ring is the weld bead and no oxide was formed around this area. And neither the thermal affected zone nor hydride formation was found in this area, whereas several small flaws could be found in the rim of inner weld bead of end plug.

V '

••'" 325 K.'

! '//

Fig.l7-a Fig.l7-b Fig,17-c Fig. 17. Micro-hardness results of K-rod at 275 and 1,580 mm Microscopic examination of fuel pellet of K-rod was performed by selecting several specimens from the rod (Fig. 17). The micro-stractures of the pellet irradiated at the lower part of fuel showed about 8 M m of grain size, and the structure of the whole area showed very similar results to the un-irradiated ones. But the structure between 810—1,580 region shows a little bit bigger grain growth rather than that of the normal irradiated fuel pellets. And a large

- 275 - JAERI-Conf 99-009 concentric ring type of grains seen in the middle of fuel pellet was identified as a agglomeration of columnar grains which were believed to be formed by the subsequent mechanisms of stoichiometry changes of UO2 affected by the coolant intrusion. It is reported that the increasing of O/U ratio up to 2.1 used to directly contribute to about 40% of thermal conductivity reduction. These postulations can be supported by the hardness test results of pellet. Fig. 17-a and 17-b show the micro-hardness distributions. Fig. 17-b shows a little bit higher hardness numbers than the ones of 17-a, which means the increasing of O/U ratio due to coolant intrusion and subsequent oxidizing of UO2 were made in comparatively high temperature environment. The dark area showing about 30 of hardness number are the resin mount which are penetrated through the pores in the center part of pellet during specimen preparation. A large amount of pores possessed by the resin mount can explain that the temperature of this region was very high compared to the other clean area of fuel rod. Oxides formed inside and outside of fuel cladding tube were measured for specimens selected different 8 locations. Overall oxides thickness distributions are showing 3~ 10 times thicker values in inside than outside. No oxide formation was seen in both end parts of fuel rod and about 3 //m of uniform oxides layers were seen between 1,300 — 3,000 mi region. In case of the oxides formed inner side of clad, maximum thickness of 11.25 nm oxides region was found around the defect area at 1,300 mm and in the remaining part of the rod up to 3,300 mm region, about 10 ft m of oxides were uniformly distributed.

SUMMARY

Rapid increases of Iodine-131 activity were detected two times during test operation of plant in the end of July and in the middle of August. Considering that the first Iodine activity peak was happened irrespective of plant power changes and a part of fission plume was found just upper part of the lower defect, it was believed that the first peak was contributed by the defect made in the lower part of R-rod. And considering the power decrease from 80% to 30% when the second Iodine peak was occurred, it was believed that the hydrided cladding tube of K-rod was failed by the thermal stresses acted on the clad accompanied with the power transients. A series of non-destructive and destructive hot cell examination have been performed for the rods which were irradiated at the initial core of nuclear power plant. Two rods, notified as R- and K-rod were identified as defective fuel rods through the on-site inspection and transferred to post irradiation examination facility (PIEF) at KAERI to investigate the root causes of fuel rod failure and to establish subsequent remedies to prevent similar failure

- 276 - JAERI-Conf 99-009 occurrences in reactor. A precise PIE for the R-rod shows that the failure of this rod was oriented from the debris induced fretting mechanism made by a foreign materials with very sharp and hard end tip. A very hard and sharp tip of debris trapped in the first spacer grid spring shell made a continuous pressure onto the fuel cladding tube until the through hole debris induced fretting failure was made. This is the primary root cause of failure of R-rod. The final conclusion of failure cause of K-rod could be made as a random hydride failure which might probabilistically be occurred under the normal Q/C and Q/A activities implied in the fuel fabrication process. Even though the exact route for the hydrogen intrusion from outside was not identified, there were not any evidences to exclude the existence of hydrogen sources in the fuel pellets or inside the cladding tube. But, despite of the above random hydride failure conclusion, the possibility of secondary hydride failure originated from the end plug failure could not be excluded with the consideration of the shape, size, orientation and location of defect existed in the end plug matrix material.

REFERENCES

[1] Seung-Gy Ro, Eun-Ka Kim, Key-Soon Lee, Duck-Kee Min, "Post-irradiation examination of Kori-1 nuclear power plant fuels," J. of Nuclear Materials 209 (1994) pp.242-247

[2] F. Gazarolli and H. Stehle, "The main causes of fuel element failure in Water-cooled power reactor," Atom. Ener. Rev., 17(1979)31

[3] H. Stehle, "Uranium dioxide properties for LWR fuel rods," Nuclear engineering and design, 33(1975)230.

[4] D.R.Olander and S.Vankin, "Secondary Hydriding of Defected Zircaloy-Clad Fuel Rods," EPRI-TR-101773, Univ. of California, Berkeley (1993)

[5] H. Kunishi, H.W.Wilson and R.N.Stanutz, "Evaluation of Fuel Rod Leakage Mechanism- Summary Reports," PRITR-104721, Westinghouse Electric Corporation (1994)

- 277- i JP9950647 JAERI-Conf 99-009 |

3.6 HYDRIDING FAILURE ANALYSIS BASED ON PIE DATA

Yong-SooKim

Department of Nuclear Engineering, Hanyang university, Seoul 133-791, Korea

Hyun-Taek Park, Hwee-Soo Jun

Fuel and Reactor Engineering, Nuclear Power Generation Department, Korea Electric Power Corp., Seoul 689-880, Korea

Yong-Bum Chun, Gil-Sung You, Duck-Kee Min, Eun-Ka Kim, Seung-Gy Ro

Nuclear Fuel Cycle Development Korea Atomic Energy Research Institute, Taejon 305-600, Korea

ABSTRACT

Failure causes of the two fuel rods of a Korean nuclear power plant had been investigated by using PIE technique. The destructive and physico-chemical examinations revealed that the clad hydriding phenomena had caused the rod failures primarily and secondarily in each case. In this study the basic mechanisms of the primary and the secondary hydriding failures are reviewed, PIE data such as cladding inner and outer surface oxide thickness and the restructuring of fuel pellets are analyzed, and they are compared with predicted behaviors by a fuel performance code. The results strongly support that the hydriding processes, primary and secondary, had played critical roles in the respective fuel rods failures.

1. INTRODUCTION

One of the frequent fuel failures in light water reactors is hydrided or hydriding- related failure. When a reactor fuel element is defective during operation, cladding no longer provides a barrier between the fission-induced burning fuel element and the coolant. The presence of this defective fuel may present economic penalties to the power utility. Sometimes, severe secondary damage can follow the primary failure: the existing leak path can let the coolant enter the element, the coolant flashes into steam, and then complicated processes such steam oxidation of UO2 and cladding hydriding of the clad inner surface, restructuring of UO2, etc. are developed, ending up with catastrophic failure. Recent investigations have provided a better understanding of the failure processes, physical and chemical.

278- JAERI-Conf 99-009

A few years ago two fuel rods were failed during cycle 1 start-up operation at the protype Korean standard nuclear power plant. Through the post irradiation examination it was revealed that the root-cause of one fuel rod is internal hydriding and the other was additionally damaged due to secondary hydriding. These findings are supported by the following analysis in this paper.

2. FAILED FUEL ROD EXAMINATION BY PIE

The two failed fuel rods were transported from the storage pool in the site to PIE facility in KAERI. The examinations, non-destructive, destructive, and chemical, were carried out in the hot cells. Through the PIE, whole rods were thoroughly inspected using telescope and then oxide thicknesses of clad inner and outer surface, structural change of UO2 pellet, and hydrogen content in the clad were measured.

3. RESULTS AND DISCUSSION

Primary (Internal;) Hydriding Failure of Fuel Rod D103-K2 Hydrogenous impurities inside a fuel rod will ultimately hydride the Zircaloy cladding regardless of their initial chemical state. Massive localized hydriding leads to hydride blisters, where the volume change is visually evident on the outside of the fuel rod, to deterioration of the mechanical properties of the clad so that splits can easily develop, and eventually to perforation of the clad after local breakthrough. The main source of the hydrogen in the typical fuel rod failures caused by hydriding is the residual moisture in the UO2 fuel pellets. In the primary internal hydriding process, the residual moisture (steam) oxides the inner surface of the clad and the extent of oxidation, i.e., thickness of oxide, over the whole length of the rod just follows the axial temperature profile along the rod since there is no external source of oxidant in this case and the Zircaloy oxidation is an activated process. Figure 1 a) and 1 b) show that the inner and outer oxide thickness profiles in the fuel rod D103-K2 are in good agreement with the temperature profiles predicted by the fuel performance code, GT2R2 [1]. The code simulation is based on the nuclear design report for the fuel cycle of the unit [2]. High temperature inside the fuel pellet, especially during start-up operation, and oxidizing environment in the moisture-rich environment induce fast restructuring of the pellet micro- structure, i.e., grain growth and stoichiometry changes, etc. These phenomena are also consistent with the fuel centerline temperature profile predicted by the code (Figure lc and Figure 2).

Secondary Hydriding Failure of Fuel Rod B208-R8 Occasionally, small primary defect leads to heavy secondary hydride formation. During the initiation stage, coolant enters the fuel rod through the defect and flashes into steam. Once the internal and external pressures have equalized, steam oxidizes the internal Zircaloy cladding surface into ZrO2, resulting in the release of hydrogen. As the gases react in the fuel-cladding gap, the concentration of hydrogen continuously increases while steam is depleted. Thus, the ratio of H2/H2O increases rapidly in the gap. In the secondary hydriding process, molecular diffusion of the steam in the gap is required, that is, the steam must be supplied from the

- 279 - JAERI-Conf 99-009

primary defect site for the oxidation to be continued along the rod axis. If the ratio of H2/H2O exceeds a certain critical value at a certain elevation and the conditions for the accelerated hydriding is achieved in the region, such as protective oxide-damaged and surface flawed, then, massive hydriding can instantaneously take place thus breaches the mechanically- degraded cladding. In general, therefore, it is believed that the inner surface oxide is thickest at the primary defect site and gradually decreases when it gets far from the primary defect point. However, it is not true if temperature is varying along the rod since temperature plays the most significant role in the Zircaloy oxidation kinetics. In this failed fuel, fuel performance code predicts that temperature profile has a maximum above mid-point. Therefore, instead of gradual decrease from the primary defect site, the thickness of the inner surface oxide is increasing, following the temperature profile (Figure 3). This oxide profile and the results of the restructured pellet examination are consistant with the axial power profile of the rod (Figure 4).

Enhanced Oxidation and Remarkable Grain Growth In Figure 1 and 3 it is seen that the oxide in the neighborhood of the defect is thicker than those in other regions. It is known that zirconium alloy oxidation kinetics is enhanced under the hydrogenous environment with high H2/H2O ratio. The unusual oxide thickness near the defect may be ascribed to this hydrogen-rich environment (Figure 5). Remarkable columnar grain growth is observed in the pellet a few mm inside the periphery (Figure 2 and 4). This unexpected restructuring is found only at the elevation of highest power even under the steam-rich environment over the whole inside rod. It is known that UO2 oxidation kinetics is accelerated in the oxidizing environment as in this case. This means, therefore, that oxygen supply to the restructured spots by diffusion through the matrix was limited. In actual, the unusual grain growth under oxidizing environment is accompanied by the stoichiometric change of the pellet into UO2+X [3,4].

4. CONCLUSIONS

PIE data analyses confirm that fuel rod D103-K2 was failed by internal hydriding and the fuel rod B208-R8 was additionally damaged by secondary hydriding. The data also support the proposed mechanism for the defective fuel behaviors such as hydriding-enhanced corrosion and involvement of a certain critical ratio of H2/H2O in the secondary hydriding.

REFERENCES

[1] M.E. Cunningham and C.E. Beyer, NUREG/CR-3907, PNL-5178, Pacific Northwest Laboratory (1984) [2] KAERI and ABB/CE, Nuclear Design Report for Yonggwang Unit 4 Cycle 1, Rev. 0 (1995) [3] B.J. Lewis, F.C. Inglesias, D.S. Cox, and E. Gheorghiu, Nucl. Technol. 92 (1990) 353-362 [4] I. Amato, R.L. Colombo, and A.M. Protti, J. Amer. Ceram. Soc, 46 (1963) 407

- 280 - JAERI-Conf 99-009

370

1000 2000 3000

600 1000 2000 3000 Rod height from bottom(mm)

Figure 1. Oxide Thickness Profile and Fuel Centerline Temperature in Failed Fuel Rod D103-K2

- 281 JAERI-Conf 99-009

'*•*'•-

#5grd 1648n m D103 - K2 (275mm) (A) (B)

hyi Irided region

hyc rided (fla :e-off) 13103 Y.I (A) (B)

#3gnd 850m n

K2n.l60mr.i) (A)' (B)

\ ,

A ..

•) ),.*,.• >*, •4- .-•> #lgrd 4 88mm vv.vv- :; D103 - K2 (1,300mm) (A) (B)

Figure 2. _ "- A ' 8 c Micro-structural ,\ Change of UO2 ;V4

D103 -K2 (2,100mm) (A) (B)

- 282 JAERI-Conf 99-009

370 O

1000 2000 3000 440 12- point of defect I o° - 420 CD o I o 9- - 400 a. CD B •a - 380 6- / O CD o 0) / oxidation enhanced - 360 O / region I 1 3- in / 340 c a> c c 1 0- 320 O 1000 2000 3000 4000

1600-

1400-

1200-

1000-

800-

600 1000 2000 3000 Rod height from bottom(mm)

Figure 3. Oxide Thickness Profile and Fuel Centerline Temperature in Failed Fuel Rod B208-R8

- 283 - JAERI-Conf 99-009

hy irided

ABC

#8 grid -» •." •" -S.' 2846n m

>y^led B208-R8(87mm) (A) (B)

#6grii 2047mm

l'208 ]*!'. f (A) (B)

I? / '•>

#4grii 1249mm

B208 - R8 (1,300mm) (A) (B)

#2gril 450mm

pnmary B208 -¥8 (27lOOmm) (A) (B) defect

M Figure 4. Micro-structural Change of UO2

- ' • K 1 B208 - R8 (2,900mm) (A) (B)

- 284 - JAERI-Conf 99-009

30- Ml ' I i • r

25-

20

P IP =103

r I// 600 1200 1800 2400 6000 6600 7200 7800 Time (min.)

Figure 5. Zircaloy Oxidation Enhancement in Hydriding Environment

l:il^

S4f

* i

/ ft \

3 /i

•;f •'• f**\ : magnified in right UO2 Radial Direction Figure 6. Columnar Grain Growth in Steam Oxidation Environment

- 285 - JAERI-Conf 99-009 JP9950648

3.7 RE-IRRADIATION TESTS OF SPENT FUEL AT JMTR

BY MEANS OF RE-INSTRUMENTATION TECHNIQUE

Jinichi Nakamura, Michio Shimizu, Yasuichi Endo, Hideaki Nabeya, Kenichi Ichise, Junichi Saito, Kunio Oshima and Hiroshi Uetsuka

Japan Atomic Energy Research Institute Tokai-mura, Naka-gun, Ibaraki-ken,JAPAN

ABSTRACT

JAERI has developed re-irradiation test procedures of spent fuel irradiated at commercial reactor by means of re-instrumentation technique. Full length rods irradiated at commercial LWRs were refablicated to short length rods, and rod inner pressure gauges and fuel center thermocouples were re-instrumented to the rods. Re-irradiation tests to study the fuel behavior during power change were carried out by means of BOCA/OSF-1 facility at the JMTR. In the tests to study the fission gas release during power change, the rod inner pressure increase was observed during power change, especially during power reduction. The fission gas release during power reduction is estimated to be the release from fission gas bubbles on the grain boundary caused by the thermal stress in the pellet during power reduction. Re-irradiation test of gadolinia added fuel was performed by means of dual re- instrumentation technique (fuel center thermocouples and rod inner pressure gauge). A stepwise fission gas release during power change, and the following fuel center temperature change due to gap conductance change were observed.

INTRODUCTION

The discharged burnup of LWR fuel assemblies has been increased step by step in Japan and other countries in order to reduce the fuel cycle costs and the amount of spent fuel. It sometimes takes long time to attain high burnup for test rod in some test reactor, and the re- irradiation tests of commercial spent fuel at test reactor are preferable to study the fuel behaviors at high burnup also from the view point of the irradiation conditions during base irradiation.

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The increase of fuel burnup means the increase of fission gas accumulation, and the increase of fission gas release may result in the increase of inner pressure of fuel rod beyond the system pressure. Therefore, there is some concerns about the effects of load following operation or power change on the fission gas release. Fission gas release during power change of CANDU fuel was studied by Notley and MacEvan[l]. They observed inner pressure increase during power change, and attributed this inner pressure increase to fission gas release caused by thermal stress. Kogai et al.[2] performed load following tests and observed inner pressure increase during power change. They attributed the inner pressure increase to the fission gas release from fission gas bubbles on grain boundary. They proposed that the maximum fission gas contained at grain boundary is controlled by static pressure in the pellet due to PCMI, and that fission gas release from fission gas bubbles on grain boundary occurs during power reduction caused by the reduction of static pressure in the pellet. Rawland et al.[3] also performed fuel irradiation tests under load following and simulated Automatic Frequency Control (AFC) operation. These tests used small gap rods, and the effects of power change on fission gas release of large gap rod have not been studied yet. Therefore, the fission gas release of large gap rod during power change was studied at the JMTR by means of re-instrumentation of rod inner pressure gauge to the fuel rods irradiated in commercial reactor. On the other hand, the gadolinia concentration in pellet to reduce the excess reactivity at the beginning of fuel assembly irradiation is gradually increasing with the extension of fuel burnup at LWRs. The thermal conductivity of gadolinia added fuel is lower than that of normal UO2 fuel, and the thermal performance of gadolinia added fuel is also one of the important phenomena in the fuel behavior. The JMTR has recently developed re- instrumentation techniques of fuel center thermocouples and rod inner pressure gauge to pre- irradiated fuel[4], and the re-irradiation test to study the thermal performance and fission gas release of dadolinia added fuel has been performed.

FISSION GAS RELEASE TEST DURING POWER CHANGE

1. Experimental methods A 7x7 BWR type rod irradiated at Tsuruga unit 1 reactor up to 22MWd/kgU was used for the test. Detailed PIE results on the sibling rods were reported in literature[5]. Puncturing test and non-destructive tests were performed on the rod. Then, five rods of about 40 cm length were cut from the flat power profile position between the spacer of the full length rod in the hot laboratory in JAERI, and some pellets were removed from the both ends of the short rods. Then new end plugs were welded at the both ends of the short rods, and the rod inner pressure gauge was welded at one end of the each short rod. Arc charge was used to

- 287 - JAERI-Conf 99-009 perforate the wall between the rod inner pressure gauge and the rod plenum. The specification of the four rods used in the tests is listed in Table 1. The rods was installed in BOCA(Boiling Water Capsule) and reirradiated in OSF-1 at the JMTR. The details of in-core part of BOCA/OSF-1 are shown in Fig.l. The power of the rod was measured by coolant temperature increase between the inlet and outlet of the OSF-1, which had been calibrated by a heater capsule just before the irradiation tests. The accuracy of the power calibration was estimated within ± 5%. The power of the rod was controlled by pressure change of He-3 gas contained in He-3 screen in OSF-1 just around the BOCA. The principle of the present test is a comparison test of fission gas release under different operational modes. The main modes are depicted in Fig.2, i.e., steady state, power cycling, and daily load following operations. The maximum power level and the total operation time at that power level in each operation mode were adjusted to the same values for comparison. Beside that, one rod was used to investigate the effects of power level on fission gas release during power change.

2. Test results & discussion Figure.3 shows the rod power and rod inner pressure change during steady state operation. The rod was conditioned at 20 kW/m for several hours, and the rod power was increased stepwise up to 40.5 kW/m and kept for 84 h. The rod inner pressure increased gradually during high power period, and the inner pressure suddenly increased during the power reduction after the high power period as shown in Fig.3. The initial diameter gap of this rod was 310 fim and the calculation of fuel behavior analysis code FEMAXI-1V[6] showed that the PCMI is very small even at the maximum power. The inner pressure at the maximum power level increased continuously as shown in Fig.3, and such a continuous increase of inner pressure suggests that the gap was open even at the maximum power level. Therefore, the rod inner pressure increase during power reduction is estimated to be caused by fission gas release from pellet inside and not by opening of the closed gap during power reduction. The rod power and the rod inner pressure change during a power cycling test are depicted in Fig.4. The rod power was increased stepwise from 20 kW/m to 40.5 kW/m, and then the rod was irradiated under power cycling mode. The rod inner pressure increased during power cycling, especially during rod power reduction. The pressure increase at power cycling depends on the length of the high power operation period just before power reduction and long high power operation period resulted in large pressure increase at power reduction as shown in Fig.4. At the end of the test, power cycling of short interval was repeated, and the inner pressure increase during each power reduction was gradually getting small with time. The rod inner pressure change of the rod during the third power reduction period, in which largest pressure increase was observed, is depicted in Fig.5. The measured inner

- 288 - JAERl-Conf 99-009 pressure showed increase during the power cycling. However, at the low power level the decrease of fuel temperature and the increase of free volume result in rod inner pressure decrease for the same amount of fission gas released in the free volume in the rod, and it becomes difficult to distinguish whether the fission gas release occurred during power reduction or during power increase. The rod inner pressure under 40.5 kW/m condition was estimated for power cycling period and also depicted in Fig.5. The estimated pressure under 40.5 kW/m showed that the fission gas release during power cycling occurs mainly during power reduction and not during power increase. A simulated daily load following operation test was also carried out. The rod power was kept at 40.5 kW/m during high power operation and at 20 kW/m during low power operation. The load follow operation mode was 14h-lh-8h-lh type simulating the daily load follow concerning time, but the rod power during high power operation was considerably higher than that at a commercial reactor. The rod inner pressure increased during high power operation and during power reduction, and the tendency was similar to the power cycling test, mentioned above. These three modes were repeated two times using the same rods, respectively. The rod inner pressure changes are plotted in Fig.6 as a function of the total holding time at 40 kW/m. The inner pressure of steady state rod increased continuously during high power operation and also increased stepwise at power reduction after the first and the second tests and at the unscheduled shutdown of the reactor. The inner pressure of the power cycling rod showed stepwise increase at power reduction. The inner pressure of load following rod also showed stepwise increase during power reduction. To study the effects of the rod power level on fission gas release during power cycling, one of the shortened rods was irradiated in BOCA in the mode shown in Fig. 7. The rod power level was increased stepwise from 30 kW/m to 40kW/m, and steady state operation and power cycling operation were repeated at each power level as shown in Fig.7. Total holding time at each high power operation during power cycling was 22 h and same as that during steady state operation. The inner pressure gradually increased and pressure increase was more prominent at the higher power level. The pressure increase during power cycling is larger than that during steady state operation at each power level.

In the present test, the rod inner pressure increased during power change, especially during power reduction. Such inner pressure increase during power reduction is expected to occur due to the opening of the closed gap or reduction of PCMI in case of a small gap rod. In a small gap rod, the gap closes at high power operation and the fission gas, released from pellet to gap, cannot reach plenum or pressure gauge during high power operation. On the other hand, under strong PCMI, the maximum amount of fission gas accommodated on the grain boundary depends on the compressive stress in the pellet, and fission gas is released during power reduction due to the decrease of the maximum amount of fission gas

- 289- JAERI-Conf 99-009 accommodated on grain boundary. However, the rods used in the present tests have large gap of 310 /im and the PCMI is estimated to be very small even at the high power level of 40 kW/m by means of the calculation of fuel behavior analysis code FEMAXI- IV [6]. Therefore, the inner pressure increase during power reduction is estimated to be caused by the fission gas release which originated from the pellet inside during power reduction irrelevant to PCMI. The second feature of the inner pressure increase during power reduction is the dependence of the pressure change on the holding time just before the power reduction as shown in Fig.4. The pressure increase during power reduction after a long holding period at high power is larger than that after short holding time. The estimated fission gas release from the inner pressure increase are shown in Fig.8. The fission gas release occurs stepwise at power reduction in each mode, however, generally the rate of the fission gas release is proportional to the square root of the total holding time at 40 kW/m. These dependencies on time suggests that diffusion process dominates the fission gas release. These time dependencies also suggest that the fission gas release during power reduction is from fission gas bubbles on the grain boundary, because the amount of the fission gas arrives at grain boundary is almost proportional to the square root of the holding time at high power and some parts of the fission gas on the grain boundary seems to be released at accelerated release rate during power reduction. A possible explanation of fission gas release during power reduction is as follows: During the base irradiation, fission gas is generated in the pellet and diffuses through the grain to grain boundary. At high power operation, grain growth occurs and the fission gas is swept out and accumulated at grain boundary. The fission gas bubbles on the grain boundary grow gradually and interlinkage of fission gas bubbles result in the formation of open porosity and fission gas release. The stress around pellet center at high power is compressive, and it decreases gradually during holding time at high power due to relaxation or creep of pellet at high temperature. At power reduction, the stress around pellet center changes from compressive to tensile due to temperature decrease, and the tensile stress at grain boundary may promote the fission gas bubble growth or bubble interlinkage on the grain boundary. Micro cracks through the grain boundary or formation of open porosity may occur, and the fission gas released from grain boundary bubbles into the free volume in the rod is estimated to result in the inner pressure increase during power reduction. The fission gas release rate during power cycling operation was larger than that during steady operation between 30kW/m and 40kW/m. A possible reason of the difference may be as follows: The fission gas in the bubbles on the grain boundary is released during power reduction due to thermal stress, and the gap conductance of the rod decreases due to the fission gas release. Then the pellet temperature increases and the diffusion of fission gas becomes fast. This results in the increase of fission gas, which reaches at grainboudary bubble or microcrack.

- 290 - JAERI-Conf 99-009

The fission gas release during power reduction was prominent at high power such as 40 kW/m. In case of commercial reactor, the rod power is lower than the power level of the present test, and generally decreases with burnup, and the fission gas accumulation rate on the grain boundary is relatively small. Therefore, the power cycling in commercial reactor may have minor effects on fission gas release of the fuel rod.

RE-IRRADIATION TEST OF GADOLINIA ADDED FUEL

1. Experimental methods A 17X17 PWR type fuel rod added with 6 wt% gadolinia was irradiated at Ohi unit 2 reactor up to 24MWd/kgU. The rod was transported to the hot laboratory in JAERI at Tokai. Puncturing test and non-destructive tests were performed on the rod. Then, a rod of about 25 cm length was cut from the flat power profile position between the spacer of the full length rod, and refablication of short rod was performed by the similar ways mentioned in the previous section. The rod was transported to the hot laboratory of the JMTR and the re- instrumentation of fuel center thermocouples was performed. The re-instrumentation technique of fuel center thermocouples was developed at the JMTR[4]. Figure 9 shows the the procedures of fuel center thermocouple re-instrumentation to irradiated fuel rod. The fuel rod was set in the double container of the drilling machine, and the container was pressurized with 1 MPa carbon dioxide(CO2) gas. Then, the CO2 gas was cooled by liquid

N2 to fix the fuel pellets with frozen CO2. The center hole of the fuel was machined with diamond drill, and the drilling and cleaning by vacuum were repeated several hundred times.

Finally, a center hole of 2.5 mm in diameter and 36.6 mm in depth was machined. CO2 gas was baked out in vacuum at 300°C for 24 hours. A molybdenum tube was inserted to the hole to protect the hole wall. Then, dual instrumentation device consist of fuel center thermocouples (W5Re-W26Re, outer diameter of the sheath: 1.8mm) and rod inner pressure gauge was installed and welded to the rod. The dual instrumentation device is shown in Fig. 10. The specification of the rod reinstrumeted with fuel center thermocouples is listed in Table 2. The rods was installed in BOCA and reirradiated in OSF-1 at the JMTR same as the previous section. The rod was operated at first under steady state condition, and then operated under power cycling conditions. The maximum power of the rod was set to 340W/cm and the fuel center temperature and rod inner pressure during the test were measured.

2. Test results & discussion Figure. 11 shows the fuel center temperature and rod inner pressure change during the test[7]. The rod was operated under steady state condition (340W/cm, 84 h), and under

- 291 - JAERI-Conf 99-009 power cycling conditions between 340-210W/cm(high power holding time : 14 h or 2 h). The maximum power of the rod decreased about 10% during the short power cycling test due to the change of the flux distribution in the reactor core. The local linear heat rate at the fuel center thermocouple position was estimated to be about 275 W/cm during the maximum power operation. The fuel center thermocouples showed about 1160°C during the maximum power operation. After the steady state operation, the rod was operated under power cycling condition. The fuel center temperature increased about 20°C after the power reduction, and the temperature gradually returned back to the previous value with time. The inner pressure of the rod increased gradually during the high power operation from about 0.25 MPa to about 0.58 MPa. The rod inner pressure also increased during power change after the steady state operation. The initial gap of the rod was 170 fi m and the cladding crept down about 50 fi m during base irradiation. The calculation of fuel behavior analysis code FEMAXI- IV [6] showed that the gap is nearly closed but that PCMI is very small even during high power operation. Therefore, the inner pressure increase during power change of the gadolinia added fuel rod may be due to the fission gas release from grain boundary bubbles during power reduction caused by thermal stress or due to the opening of the closed gap. Anyhow, some fission gas was released during power change to free volume and gap. The decrease of gap conductance due to fission gas release during power change may have resulted in the temporally increase of fuel center temperature increase observed in the present test.

Similar test of standard UO2 fuel with fuel center thermocouples and rod inner pressure gauge will be performed in April 1999 for the comparison with the gadolinia added fuel rod.

CONCLUSIONS

JAERI has developed re-irradiation test procedures of spent fuel irradiated at commercial reactor by means of re-instrumentation technique. Re-irradiation tests to study the fuel behavior during power change and thermal performance of gadolinia added fuel were carried out by means of BOCA/OSF-1 facility at the JMTR. In the tests to study the fission gas release during power change, the rod inner pressure increase was observed during power change, especially during power reduction. The fission gas release during power reduction is estimated to be the release from fission gas bubbles on the grain boundary caused by the thermal stress in the pellet during power reduction. Power cycling operation accelerated the fission gas release compared with steady state operation at the high power levels between 30 and 40 kW/m. Re-irradiation test of gadolinia fuel was performed by means of dual re-instrumentation technique (fuel center thermocouples and rod inner pressure gauge). A stepwise fission gas release during power change, and the following fuel center temperature change due to gap conductance change were observed.

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REFERENCES

1. M.J.F.Nortley and J.R.MacEwan, Nucl.App.2(1966)477 2. T.Kogai et al., J. Nucl. Mater. 158(1988)64 3. T.Rowland et al., International Topical Meeting on LWR Fuel Performance, Avinion, April (1991) 4. M.Shimizu et al. JAERI-Tech 95-037(1995) 5. Y.Tsuchie et al., J. Atomic Energy Society of Japan 29(1987)219(in Japanese) 6. M.Suzuki & H.Saitou, JAERI-Data/Code 97-043(1997) 7. J.Nakamura et. al., 'Re-irradiation test of gadolinia added fuel', paper presented at the annual meeting of AESJ, Hiroshima,22nd-25th,March 1999. Table 1 Specification of shortened BWR rod

• cladding outer diameter 14.3mm • cladding thickness 0.81 ± 0.08mm • pellet diameter 12.37 ± 0.03mm • gap width 310 //m • stack length 229-315 mm • density 94-95 %TD • enrichment 2.79 % • burnup 22.5-25.6 MWd/kgU • initial grain diameter ~ 5 /z m • FGR during base irradiation ~ 0.4%

Table 2 Specification of shortened PWR rod

• cladding outer diameter 9.50 ± 0.04mm • cladding inner diameter 8.22 ± 0.04mm • pellet diameter 8.05 ± 0.01mm • gap width 170 Aim • gadolinia concentration 6wt% • enrichment 1.7% • stack length 232 mm • depth of center hole 36.6 mm • density 95 %TD • burnup 28 MWd/kgU

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Figure 1. inlet TC Details of in-core part pressure tube ofBOCA/OSF-1. BOCA capsule partition wall quick connector (socket) quick connector instrumentation (Plug) device

He-3 gas screen SPND

fuel rod (fuel stack)

shroud in-core tube outlet TC

(a) Steady state operation

40

| 30

(b) Power cycling operation 4h4h 40h 4h 20h 2h

(c) Daily load following operation 14h i4h

Time Figure 2. Different operational modes.

- 294 - JAERI-Conf 99-009

0 0 24 48 72 96 120 144 168 Time (h) Figure 3. Rod inner pressure change during steady state operation.

3.6 1 1 i 80

3.0 -6- 0 CO Rod LHR Q. 40kW/m ^2.4 •A, .' <—l»rir- 40 a: i (A 20kV//m /IP -fa —•—' ' ill- "*L §.1.8 Tl 1 20 CO -e o Q_ C —o Rod pressure mnl ~~ 1 12 0 OH 0.6h

0 i i i t 0 24 48 72 96 120 144 168 Time (h) Figure 4. Rod inner pressure change during power cycling operation.

- 295 - JAERI-Conf 99-009

1.6 LHR of fuel rod flj 40kW/m Q_ 20kW/m

§1.4 estimated inner (A pressure at (A \40kW/m,'

0) 1 XI \ measured o inner pressure 1.0 0 30 60 90 120 Time (min ) Figure 5. Rod inner pressure change during the third power cycling operation. 3.5i ? • < 1

3.0

33XFCK £2.5

daily load follow 3 S2.0 operation^ a 27XFCR Q.

= steady state operation

1.0

0 50 100 150 200 250 300 Total time operated at 40 kW/m ( h ) Figure 6. Rod inner pressure change under different operational modes as a function of holding time at 40 kW/m.

- 296 - JAERI-Conf 99-009

50 40 kW/m 30 kW/m 35 kW/m 25 I steady power steady power steady power cycling state cycling state cycling state 2.0 CO Q. 1.5

3 | 1.0 Q.

•i 0.5 XI o 0 0 20 40 60 80 100 120 140 160 180190 Time ( h ) Figure 7. Rod inner pressure change during power cycling operation at different power levels(30,35,40kW/m). 100r . 1 . • • . ••) 1 r-

60 40 power cycling 30 daily load follow operation ^ operation 20 f^ "\ power reduction co steady state I operation at 10 *-- • 1 power reduction o

• i . ,_,± 10 20 40 60 100 200 300400 Total time operated at 40 kW/m ( h ) Figure 8. Estimated FGR under different operational modes as a function of total time operated at 40 kW/m.

- 297- JAERI-Conf 99-009

•=>

Cutting Freezing | Drilling Removing ol UO2 Chips

Dual Instrumentation^ 0 Device 11 In n n nil : 1 1 N? 11 u V U Ul 1 <=•

Inserting of Sleeve Welding Baking Out Thermocouple Inserting

Figure 9. Procedures of thermocouples re-instrumentation to irradiated fuel rod.

Pressure Gage

Quick Connector Differential (plug) Transformer Ml Cable Bellows! Zry/SS Friction Joint Thermocouple!

to Quick Connector Hermetic Connector to Fuel Rod (socket) in BOCA End Plug

Figure 10. Dual instrumentation device for measurement of fuel center temperature and internal pressure of fuel rod.

- 298 - JAERI-Conf 99-009

1500 2.4

fuel center temperature

TO 2> 1000 1.6 CL 2

o. (/) (A E 0)

Q) d c § 500 0.8 •oo a: start of pressure measurement

0 0 100 200 300 400 Time (h )

Figure 11. Fuel center temperature and rod inner pressure change of gadolinia added fuel rod.

- 299- JAERI-Conf 99-009 JP9950649

3.8 HANARO FUEL GAMMA SCANNING

Kwon-pyo HONG, Tae-yon KIM, Dae-gyu PARK, Dae-seo KOO IMEF Department Korea Atomic Energy Research Institute Yuseong-Ku, Taejon, Korea

Bong-goo KIM Hanaro Center Korea Atomic Energy Research Institute Yuseong-Ku, Taejon, Korea

Abstract

One bundle of Hanaro fuel irradiated up to 50%-burnup and cooled for 6 months was transported to IMEF for PIE, which has 6 elements. At first we measured the longitudinal distribution and the rotational distribution of several dominant peaks intensities from the bundle. After dismantling of the bundle we measured the longitudinal distribution of 137Cs and 134Cs peaks in each fuel element to see the burn-up feature. And finally we found out the relative number distribution of 137Cs and 134Cs for each detection point, which would be used for burn-up calculation. The relative detection efficiency of the scanning system was obtained experimentally by using the 134Cs peaks. We also checked up the azimuthal difference of peak intensity for each element, which are resulted about 2% of difference. These data will be used for the further analysis of Hanaro fuel performance evaluation.

Introduction

The fuel bundle used in this experiments has same dimension with the normal Hanaro fuel. This Hanaro bundle has 36 elements, but only 6 elements have fuel meat and others are dummies. It was irradiated up to the 50% of burn-up and cooled about 6 months. As one of the fuel performance evaluating program, we did gamma scanning for the bundle assembly and did also for the each of 6 elements. The fuel was transported in September 1998, and we did gamma scanning for 3 months.

- 300 - JAERI-Conf 99-009

Measurement

Measuring Equipment

The gamma scanning system of EMEF consists of bench, collimator, detector and analyzer.[l] The bench located in Ml hotcell has 2 degree of freedom of movement - vertical and rotational. The collimator used in this experiments is 2mm x 30mm slit type and the distance between fuel and detector is about 1500mm. The detector is HPGe(15% of efficiency). We had to put a lead block of 25mm thickness in front of detector to weaken the beam intensity to avoid the high dead time.

Bundle Gamma Scanning

A sample of gamma-ray spectrum we obtained is as Fig. 1. Because we are interesting of the energy region between 500keV and 1500keV, we adjusted the gain of analyzer to this purpose.

1O7

i c

O 105

1O3 :

102 1OOO 2OOO 3OOO 4OOO Channel

Fig. 1. y-ray spectrum for Hanaro Fuel.

At first we measured the longitudinal distribution and the rotational distribution of a few

- 301 - JAERI-Conf 99-009 dominant peaks. The scanning step is 10 mm in longitudinal and 2 * in rotational. In Fig. 2 the number of nuclides we can find out explicitly is 8 and the most burned position is about 1/3 location from the bottom and most of peaks distribution are same shape with gross distribution except 134Cs, which will be used for burn-up indicator. In This results are caused by the geometry of fuel elements - all of 6 elements are located at outer ring with 60 * period.

Gross Ru1O6 Cs137 Zr95 Zr95.2. Nb95 Cs134 Ce144 1O5-

c 3 0 0 (0 (D Q.

"So. 1O3-

~ «*"•-

102 2O 4O 6O 8O 1OO Height (cm)

Fig. 2. Longitudinal scanning results for Hanaro bundle(KHF-051).

- 302 - JAERI-Conf 99-009

Statiststical fluctuation for rotation of a fuel rod

15OOO-

nS

0 "6 c 3

ID a.

1OO 2OO 3OO Angle (degree)

Fig. 3. Rotational scanning results for Hanaro bundle(KHF-051)

' V V V V V • NAAAAA/^

2£. a o 0.

10* 0 60 120 180 240 300 360 Angle (degree)

Fig. 4. Rotational scanning results for an element.

- 303 - JAERI-Conf 99-009

Element Gamma Scanning After dismantling the bundle we have checked up the presence of rotational difference in each element. The difference is about 2% as Fig. 4 and this effect is considered as the irradiation flux difference in reactor core.

Longitudinal Distribution

Longitudinal distribution of 137Cs peak (661.66keV) and the largest 134Cs peak (795.84keV) are measured, where the number of measuring points are 75 with 10mm step. Fig. 5. represents that all of elements have almost same distribution.

IMEF-O1O Rod IMEF-1O1 Rod

3x10*

Cs-137(661.66 koV) • Cs-137(661.66 koV) Cs-1 34(795.84 keV) * Cs-1 37(795.84 keV)

(0 4-»

0 2x10« 2x10« o ^ A

O 1O 2O 3O 4O 5O 6O 7O 1O 2O 30 40 50 60 7O Height (cm) Height (cm)

Fig. 5. Longitudinal gamma scanning results for each element.

- 304 - JAERI-Conf 99-009

IMEF-llORod IMEF-lOORod

1 1 1 1 ' i i

• Cs-137(661.66 keV) • Cs-137(661 .66 keV) A Cs-134(795.84 keV) * Cs-134(795.84 keV)

(A 2x10" ITS, C 2x1 O< - • A // w .* + (0 s 0) v a f • a A \ ''"* 3 A • » *A 1x10" o 1x10" - I \ \ A A s \ " AA A A *A •' ^SA

m 0 O Uk O 10 20 30 40 50 60 70 0 10 20 30 40 50 60 70 Height (cm) Height (cm)

IMEF-001 Rod Oil Rod

3X10" JX1U"-

• Cs-137(661.66 keV) Cs-137(662 keV) ' •» Cs-134(795.84 keV) A Cs-134(796 keV)

B 2x10" 2x1 &•-

S Arf^A.**A "U I mm 3

A *. A % •-- / A 4A '% A "• A \ >ta l pea k co u • * ** *• I- 1x10* A 1x10"- A \ -. A \ m A •• A A • A^ * AA VS» A A/ \ " ^A A

0- 0 10 20 30 40 50 60 70 10 20 30 40 50 60 70 Height (cm) Height (cm)

Fig. 5. Longitudinal gamma scanning results for each element.(continued)

- 305 - JAERI-Conf 99-009

Analysis

Relative Efficiency

The relation between peak area and the amount of nuclide is as follows.

s = ;v(inj_)/y

where S means peak area per unit time, N is number of atoms, ^ is gamma ray emission probability per unit decay, and e is detection efficiency. For the 134Cs peaks, we can obtain Ne(E)fromeq. (1).

---(2)

I34 By least square fitting of 5 peaks of Cs, we can find N134e(E) experimentally, which is called relative efficiency. [2] In Fig. 6, the relative efficiency curve obtained from 134Cs peaks is represented.

, - .

• Spectrum A

1.O- A- Spectrum B I.I . itiv e efficienc y (0

0.2-

0.0- 400 600 8OO 100O 12OO 140O Energy (keV)

Fig. 6. The relative efficiency curve obtained from Cs peaks

- 306 - JAERI-Conf 99-009

Nuclide Number Ratio

For unknown peak, by substituting e(E) of (1) with that of (2) we obtained

» r — -(3)

So we can calculate the number ratio Nun/N134 from (3), however actually we have re- calculate the atomic number ratio to the maximum value of I37Cs. In Table 1. and Fig. 7, we presented the atom number distribution profile for 6 elements. Table 1. The relative atom number ratio of 134Cs and 154Eu to '"Cs^,,

The atom number ratio Element 627 mm 452 mm 277 mm 202 mm 127 mm IMEF-010 0.47603 0.83212 0.96111 0.90781 0.78912 IMEF-101 0.48742 0.87635 0.96977 0.88740 0.76731

IMEF-110 0.49587 0.84154 0.95361 0.88782 0.75545

IMEF-100 0.53022 0.88977 1.00000 0.92155 0.80038

IMEF-001 0.46859 0.82224 0.93726 0.86310 0.74713 IMEF-011 0.47596 0.81935 0.95063 0.90002 0.76158 IMEF-010 0.01062 0.03568 0.05102 0.04471 0.03213 (0.00028) (0.00115) (0.00100) (0.00066) (0.00029) IMEF-101 0.01070 0.03642 0.04848 0.04110 0.02869 (0.00014) (0.00056) (0.00053) (0.00079) (0.00029) IMEF-110 0.01120 0.03609 0.04961 0.04220 0.02949 (0.00012) (0.00073) (0.00089) (0.00072) (0.00072) IMEF-100 0.01241 0.03841 0.05193 0.04394 0.03099 (0.00030) (0.00109) (0.00111) (0.00121) (0.00079) IMEF-001 0.01004 0.03305 0.04630 0.03875 0.02795 (0.00025) (0.00066) (0.00123) (0.00069) (0.00084) IMEF-011 0.01038 0.03339 0.04713 0.04118 0.02862 (0.00046) (0.00099) (0.00107) (0.00126) (0.00062) IMEF-010 0.00143 0.00460 0.00646 0.00571 0.00409 (0.00005) (0.00018) (0.00017) (0.00021) (0.00011) IMEF-101 0.00139 0.00492 0.00629 0.00543 0.00390 (0.00003) (0.00011) (0.00012) (0.00015) (0.00021)

IMEF-110 0.00142 0.00489 0.00648 0.00554 0.00389 (0.00003) (0.00014) (0.00013) (0.00005) (0.00010)

IMEF-100 0.00171 0.00516 0.00696 0.00587 0.00423 (0.00009) (0.00004) (0.00009) (0.00000) (0.00016)

IMEF-001 0.00126 0.00448 0.00604 0.00513 0.00366 (0.00007) (0.00007) (0.00024) (0.00013) (0.00007)

IMEF-011 0.00140 0.00459 0.00631 0.00543 0.00377 (0.00008) (0.00013) (0.00013) (0.00015) (0.00012)

- 307 - JAERI-Conf 99-009

Nuclear number ratio to the maximum number of Cs-137 Nuclear number ratio to the maximum number of Cs-137 (IMEF-010 fuel rod) (IMEF-101 fuel rod )

t • i : • Cs-137 • • • Cs-137 A CS-134 A CS-134 r EU-1S4 T EU-154 1 - . • » 1 - . » ' 1

0.1 - ; 0.1 - i

A * A A A A

0.01 - A 0.01 - A

T 1E-3- 1E-3- 100 2OO 3OO 400 SOO 6OO 700 100 2OO 300 4O0 5OO 6OO 7OO Height (mm) Height (mm)

Nuclear number ratio to the maximum number of Cs-137 Nuclear number ratio to the maximum number of Cs-137 (IMEF 110 fuel rod) (IMEF-100 fuel rod)

I • i

• Cs-137 • Cs-137 A CS-134 A CS-134 • Eu-154 T Eu-154

1 - # 1 - 0 : • • ' ' a w 0 n E _ § 0.1- - 0.1 - c A « '• A A 0 A A o A A D Z 0.01 - A 0.01 - T T V

T T 1E-3- 1E-3H 100 200 300 400 500 600 700 100 200 300 400 SOO 600 700 Height (mm) Height (mm)

137 134 154 Fig. 7. The number ratio of Cs, Cs, Eu to Csmax. in each element.

- 308 - JAERI-Conf 99-009

Nuclear number ratio to the maximum number of Cs-137 Nuclear number ratio to th« maximum number of Cs-137 ( IMEF-001 fuel rod ) ( IMEF-011 fuet rod )

: • C«-137 • Ca-137 A Cs-134 A cs-134 • Eu-154 -v Eu-154 . • • • 1

rati o 5 1 numbe r

A 5 A * - : u 3 Nuclaa r

0.01 • A. -

•r * '•

T 1E-3 - O 1OO 2OO 3OO 4OO 5OO BOO 7OO 0 1OO 2OO 3OO 4OO BOO 8OO 700 Height (mm) Height (mm)

Fig. 7. The number ratio of l37Cs, l34Cs, l54Eu to . in each element(continued).

Conclusions

We obtained the relative distribution of a few nuclides in Hanaro irradiated fuel. This results will be used for further analysis as burn-up calculation. We are planning to do gamma scanning for another two bundles which are same fuel but their burn-ups are 80% and 90% each. And by using of standard gamma ray source we will try to get the absolute distribution of several nuclides next time.

References

[1] Kwon-pyo Hong et. al., Proceedings of the 2nd KAERI-JAERI Joint Seminar on the PIE Technology, pl37, Sept. 20-22. (1995).

[2] Kwon-pyo Hong et. al., Proceedings of the Korean Nuclear Society Autumn Meeting Vol H,p251, Oct. (1997).

- 309 - JP9950650

3.9 METALLURGICAL PROPERTIES OF POWER REACTOR

FUELS AFTER IRRADIATION

Gil-Sung You, Hang-Suk Seo, Sung-Ho Eom, Duck-Kee Min, Eun-Ka Kim, Dae-Seo Koo, Jun-Sik Ju, Nuclear Fuel Cycle Development Korea Atomic Energy Research Institute P.O. Box 105, Yusong, Taejon, 305-600, Korea

ABSTRACT

To evaluate in-reactor performance of commercial power reactor fuels, three fuel rods irradiated in Kori-1 unit in Korea were examined by the destructive examination PIE methods, such as fission gas puncturing & analysis, macro- and micro- optical microscopy, micro-hardness test, and fuel density measurement. From the analyses of the examination results, it was revealed that these fuel rods were irradiated soundly and did not show abnormal performance in reactor.

INTRODUCTION

The assessment of in-reactor performance and integrity of nuclear fuels should be based on the evaluation of the PIE data [1,2]. Especially, the destructive examinations on irradiated fuels, such as fission gas puncturing & analysis, macro- & micro-optical microscopy, micro-hardness test and fuel density measurement, can play a central role for this purpose. In this paper we have described the procedures of the destructive PIE examinations on the fuel rods which had been irradiated in Kori-1 NPP in Korea and have reported the metallurgical property data obtained from several specimens. From analyses of these data, the in-reactor performance of the fuel rods is also assessed.

- 310 - JAERI-Conf 99-009

SELECTION OF FUEL ASSEMBLY AND RODS

One fuel assembly was selected from the spent fuel storage pool of Kori-1 NPP, which is located in south seashore of Korea. And a total of 3 fuel rods from this assembly were chosen for PIE examinations. The average assembly burnup was 35.50 GWD/MTU. It had experienced 4 cycles in A8/A8/B7/D7 loading positions. The discharge date was October 24, 1986. It had been stored for about 6 years in reactor storage and PIEF pools before examination. The identification of the fuel assembly is G23 and those of three fuel rods are G23-N2, G23-I4 and G23-E3. G23-N2 fuel rod was positioned in the first low of the assembly FACE 3 and had 36.25 GWD/MTU burnup. 14 and E3 rods had 34.64 and 31.52 GWD/MTU burnup, respectively. Table 1 shows the physical characteristics of each fuel rod. The outside cladding surface of each rod looked quite clean and had numerous straight axial scratches or grooves which apparently were shallow. They might have been produced during withdrawal of the fuel rods. Generally, the lower portions of the fuel rods were uniformly dark. The upper portions of the rods had a smooth light gray to white appearance on a major portion of their surfaces. The transition zones appeared to be mottled areas of mixed light and dark coloration. The rod average diameters measured from rod axial range of 660 to 2,660 mm were 10.618 mm for N2, 10.630 mm for 14, and 10.625 mm for E3. If we assume the initial diameter (pre-irradiation value) to be the same as the diameter at top plenum area of irradiated fuel rods, the changes of diameter for each rod between before and after irradiation are -0.80, -0.81 and -0.87 %, respectively. The average ovalities for three rods are 0.013, 0.012 and 0.013 mm, respectively. The measured rod lengths were 3,882, 3,880, and 3,882 mm, respectively. The total rod length before irradiation was 3,857 mm. Therefore, the elongation lengths by irradiation are 25, 23, and 25 mm, respectively.

EXPERIMENTAL METHODS AND PROCEDURES

By the analyses of the data from non-destructive examinations, such as visual examination, gamma scanning test, eddy current test and dimensional measurement, the cutting positions and destructive examination methods on the fuel rods were determined for further detail investigation. Before cutting the rods, the three fuel rods were punctured. The released gas was collected and the volume was measured using the fission gas collection system in KAERI PIEF. The objectives of performing fission gas

- 311 - JAERI-Conf 99-009 collection and analysis were to determine if the fuel rods were failed, and to obtain the fractional fission gas release data. After fission gas collection, several sample positions on the rod were marked and cut for further detail examinations. For metallographic examination, some short rods cut from several axial positions on the rods were impregnated by resin to prevent the spalling out of the fuel fragments from cladding. After curing the resin the short rods are cut again by diamond cutting machine. For easy handling and specimen preparations the fuel rod sections were hot-mounted, ground and polished. Each specimen surface was examined both in the as-polished condition and after being etched to reveal microstructures in the fuel and hydride concentration and orientation in the cladding. Micro-hardness of the cladding materials was also measured using the optical microscope with diamond indenter. The densities of pellet fragments chosen in the several rod positions were also measured by an immersion method.

EXPERIMENTAL RESULTS

1. Rod puncturing, Fission gas collection and analysis Table 2 shows the internal gas volume, the fission gas release, and the fractional fission gas release for N2,14, and E3 rods, respectively. It was also confirmed that none of the fuel rods was failed. As shown in the table, the total gas volumes are 624.04 cc for N2, 587.44 cc for 14, and 475.38 cc for E3 at STP. The release fractions of fission gas are 1.20, 0.75, and 2.08 %, respectively.

2. Fuel Examinations 2.1 Microstructures of fuel A total of 15 samples were cut from the three fuel rods. After being etched each surface was examined. Fig. 1 shows the macro- and microstructures of transversal section at 3,002 mm position from the E3 rod bottom. As shown in the figure, there remains a lot of sintering pores in the periphery, but those are rarely observed in the center position. Another rods, such as N2 and 14 also show a similar aspect to E3. Using the pictures of fuel microstructures, we measured the grain sizes at the three different sectional positions, such as the center, the mid-radius, and the periphery. Table 3 shows the measured grain sizes at the three positions for each fuel sample. The values indicate minimum 8.0 to maximum 14.1 |im. These values are similar to the nominal design data (pre-irradiation data). Therefore, it could be concluded that there was no grain growth phenomenon in these fuel rods.

- 312 - JAERI-Conf 99-009

2.2 Density measurements on fuel pellet Table 4 shows the density measurement values on the fuel fragments selected from several axial positions for each fuel rod. The maximum value is 10.40 g/cm3 at 3,647 mm position on rod 14. The minimum value is 10.23 g/cm3 at 1,090 mm position 3 on rod E3. The density of unirradiated UO2 from nominal data was 10.40 g/cm . Therefore, it is concluded that these fuel rods had experienced the densification, but had no swelling enough to recover the original density of fuels since irradiation proceeded. Fig. 2 indicates the density distribution of the samples as a function of burnup.

3. Cladding Examinations 3.1 Oxide layers Fig. 3 shows the oxide layer thickness on the outer and inner cladding surfaces of the three fuel rods as a function of rod axial length. The outer layers were measured on all the three fuel rods, but the inner oxide layers on N2 and 14 rods only. The maximum oxide thickness is about 26 [im at 3,020 mm position on E3, and the minimum is about 6 (im at 190 mm position on 14. Fig. 4 shows the outer oxide layer appearences at the thickest position (3,065 mm from the bottom end of fuel rod) on 14. Generally, the oxide layers for all the samples are relatively uniform, but show a lot of cracks parallel to cladding. The inner oxide layers indicate about 10 Jim. Fig. 5 shows the typical inner oxide layers at 3,047 mm position from the bottom end of fuel rod N2. The inner oxide layers are not uniform, but do not have the parallel cracks like the outer oxide layers.

3.2 Hydride morphology The hydride morphology of cladding materials was inspected by metallography. Generally, it was found that the hydrides form long ribbons or bands in axial direction. Fig. 6 shows the typical hydride morphologies at several positions on rod 14. It was also found that hydride concentration at the highest temperature positions was higher than that of relatively low temperature positions. Observing the morpologies of hydrides, it can be suggested that there was no problem by hydride re-orientation in the fuel rods.

3.3 Micro-hardness For metallographic samples cut from some axial positions on each rod, the Vicker's micro-hardness tests were performed using the optical microscope with a diamond indenter. Table 5 shows the Vicker's micro-hardness values at several positions

- 313- JAERI-Conf 99-009 on each rod. No big difference was shown between these micro-hardness values. The micro-hardness values of unirradiated one were 273.3, 259.3 and 258.2 for N2,14, and E3 rods, respectively. The average values of the irradiated samples appeared 278.5, 292.2 and 288.6, respectively. Therefore, 1.9, 12.7 and 11.8 % of micro-hardness values are increased by irradiation for each respective rod.

DISCUSSIONS

From all available nondestructive data, several axial positions for each rod were selected for further detail destructive tests; The samples selected from the three rods represented a range of fuel burnups, 13.69 to 40.47 GWD/MTU. The puncturing of the rods confirmed that the rods were unfailed. The obtained data ascertained the rod integrity and showed that the fractional fission gas releases were 1.20 % on N2, 0.75 % on 14, and 2.08 % on E3. These release rates may have a big difference. Fig. 7 shows the NRC correlation, the CARO-D code prediction [3], and the present experimental data together. As shown in this figure, the fractional fission gas releases of N2 and 14 are under the correlation and code prediction, but that of E3 accords well with the value predicted by CARO-D code. Because the three fuel rods didn't show abnormal gas release rates, it could be concluded that they had experienced a normal irradiation condition in reactor. During irradiation in the reactor, the macro- and microstructures of fuel show a lot of changes according to power history, irradiation conditions, and etc. The fuel fabrication history is also important to the fuel stability during irradiation. In the investigation of fuel microstructures the fuel pellets showed no evidence of equiaxed grain growth, confirming that the fuel had operated at a low temperature condition (< 1300 °C) throughout its lifetime. No correlation between grain size and buraup was found. The thickest cladding oxide positions accord with the highest temperature positions predicted by the usual thermal analysis computer code. Because no defects were found in these fuel rods, the inner oxide layers might be formed by the oxygen from fissionning of fuel. The precipitation of zirconium hydride occurs in fuel cladding during cooling from the service temperature when the concentration of hydrogen in below the solubility limit, about 100 ppm. For hydrogen concentrations above the solubility limit, precipitation can occur during reactor operation, or existing hydride particles can dissolve and

- 314- JAERI-Conf 99-009 reprecipitate in a manner that best relieves the local stress. The hydride morphology is that of plate-let clusters arranged as long ribbons or stringers which are aligned parallel to the tube axis. The platelet width direction is aligned tangentially. Therefore, it means that the hydride might have no effects on the mechanical properties of the cladding materials.

SUMMERY

To evaluate the in-reactor performance of commercial power reactor fuels, several fuel rods irradiated in Kori-1 unit in Korea were examined by destructive examination PIE methods. The fractional fission gas releases were 1.20 % on N2, 0.75 % on 14, and 2.08 % on E3. The release rates of N2 and 14 are under the NRC correlation and the CARO-D code prediction and that of E3 accords well with the value predicted by the code. The fuel pellets showed no evidence of equiaxed grain growth, confirming that the fuel had operated at low temperature (< 1300 °C) throughout its lifetime. No correlation between burnup and positions was found. The thickest positions of cladding oxide on the three fuel rods accord with the highest temperature positions predicted by the thermal analysis computer code. The hydride platelet direction was aligned tangentially.

REFERENCES

[1] S.G Ro, et al., "Development of Post-Irradiation Examination and Evaluation Techniques for Nuclear Reactor Fuel (III)", KAERI internal report, KAERI/RR-1127/92 (1992). [2] S.G Ro, et al., "Postirradiation Examination of Kori-1 Nuclear Power Plant Fuels", J. of Nuclear Materials, 209, 242-247 (1994). [3] R. Eberle and E. Distler, "The KWU Fuel Rod Computer Code CARO", KWU Technical Report Blll/e 117/1982.

- 315- JAERI-Conf 99-009

Table 1. The characteristics of fuel rods G23-N2,14, and E3

Item Fuel Rod G23-N2 G23-I4 G23-E3 Surface Color (mm from rod bottom end) - Black 0-690 0- 630 0 - 937 - Transition 690 - 970 630- 1,171 937-1,655 - Gray 970 - top 1,171 -top 1,655-top Diameter - Average*, mm 1O.618±O.OO5 1O.63O±O.OO3 10.629±0.005 - Minimum, mm 10.604 10.618 10.619 - Diameter Change, % -0.80±0.04 -O.81±O.O3 -0.87+0.05 Ovality - Average*, mm 0.013±0.004 0.012+0.003 0.013+0.006 - Maximum, mm 0.082 0.071 0.056 Rod Length - Stack Length, mm 3,679 3,672 3,665 - Total Length, mm 3,882 3,880 3,882 * Diameter averaged over 660 - 2,660 mm. Note : Initial diameters (pre-irradiation values) are assumed to be the same as the diameter at the top plenum area of the irradiated fuel rods.

Table 2. Fission Gas Release of Fuel Rods G23-N2,14 and E3

Fuel Rod Burnup Internal Gas Fission Gas Fractional B/A (GWD/MTU) Volume (A) Release (B) Fission Gas (%) (cc, STP) (cc) Release (%) G23-N2 36.25 624.04 29.02 1.20 4.65 14 34.64 587.44 17.27 0.75 2.94 E3 31.52 475.38 43.50 2.08 9.15

- 316 - JAERl-Conf 99-009

Table 3. Grain Size of Fuel Rods G23-N2,14, and E3

Axial Grairl Size, nni Position G23-N2 G23-I4 G23-E3 (mm from Center Mid- Peri- Center Mid- Peri- Center Mid- Peri- bottom) Radius phery Radius phery Radius phery 24 11.3 12.4 11.4 ------38 ------9.8 10.2 9.6 189 9.4 8.9 8.0 14.1 11.0 9.5 - - 940 - - - 10.4 10.3 9.3 - - - 1,090 ------9.9 9.2 9.0 1,180 10.9 10.7 10.6 ------1,565 - - - 10.6 11.2 9.1 - - - 1,760 ------10.5 8.4 9.3 2,198 12.1 11.2 10.1 ------3,020 ------10.3 10.0 10.0 3,055 10.6 9.5 8.9 ------3,066 - - - 11.6 10.7 10.3 - - - 3,455 ------10.4 9.7 9.7 - - - 10.4 10.9 10.4 - - - 3,647

Table 4. Density of Fuel Pellet from Rods G23-N2,14, and E3

Axial Position Burnup Density, g/cm3 (mm from (GWD/MTU) G23-N2 G23-I4 G23-E3 bottom) 38 13.69 - - 10.32±0.01 40 16.69 10.36±0.01 - _ 190 27.32 _ 10.34±0.01 - 200 29.14 10.33+0.01 - - 940 39.17 - 10.30±0.01 1,090 35.57 _ 10.23+0.01 1,195 40.47 10.25+0.01 _ 1,565 38.06 _ 10.27±0.01 _ 3,020 33.32 10.24±0.01 3,066 36.06 10.28±0.01 _ 3,455 24.57 1O.33±O.O1 3,647 15.48 - 10.40±0.01 -

- 317 - JAERI-Conf 99-009

Table 5. Microhardness of Zircaloy Clad from Fuel Rods G23-N2,14, and E3

Axial Position Burnup Microhardness ,Hv (mm from (GWD/MTU) G23-N2 G23-I4 G23-E3 bottom) 38 13.69 - - 284.8±5.9 189 29.14 280.1+8.2 - _ 190 27.32 _ 287.2+10.8 1,565 39.39 288.5±10.3 _ _ 1,760 35.26 - 298.4+9.8 2,198 37.75 _ 299.7+7.7 _ 3,055 36.06 _ 289.6±7.3 _ 3,455 24.57 _ _ 282.5+7.2 3,647 17.00 266.8±8.7 - - Unirradiated 273.3±7.5 259.3+9.1 258.2+6.2

318- JAERI-Conf 99-009

0 C

mi tmm

1 r 4 '• -

? • •'•

CB> (0

Fig. 1. Macro- and Micro-photographs of Transversal Section at 3,002 mm From the Bottom End of Fuel Rod G23-E3.

- 319 - JAERI-Conf 99-009

10.44- • G23-N2

• O G23-I4 10.40- O A G23-E3

10.36- D I O A D '(/) 10.32- A CD o Q 10.28- o o • 10.24- A A

10 15 20 25 30 35 40 Burnup (GWD/MTU)

Fig. 2. Density Changes of Three Rod Samples as a function of Burnup.

A 24- a I 0 A 0 20- •

nicknes s | 16- 0 CD 12- D G23-N2out CO 8 . • 0 G23-I4out CD • • f A G23-E3out ~O 8- • G23-N2in 'x O A ^ t G23-I4in

4- I • I ' I • I - l ' l i 0 500 1000 1500 2000 2500 3000 3500 4000 4500 Dstance from Rod Bottom (mm)

Fig. 3. Axial Profile of Oxide Layer Thickness of Three Rods extracted from G23 Assembly.

- 320 - JAERI-Conf 99-009

Fig. 4. Oxide Layer on Outer Surface of Clad at 3,065 mm from the Bottom EndofFuelRodG23-I4.

321 - JAERI-Conf 99-009

A

C

Fig. 5. Oxide Layer on Inner Surface of Clad at 3,065 mm from the Bottom EndofFuelRodG23-I4.

- 322 - JAERI-Conf 99-009

-'.-':•-,, • '.-..I

Fig. 6. Hydride Morphology in Zircaloy Clad of Fuel Rod G23-N2. (A) 25 mm from the bottom end (B) 1,157 mm from the bottom end (C) 2,192 mm from the bottom end (D) 3,047 mm from the bottom end

- 323 JAERI-Conf 99-009

NRC CORRELATION a G23-N2 Rod o G23-I4 Rod 4- A G23-E3 Rod

CD CO 03 3 _gj (D cr CARO CODE CO 2 CD PREDICTION c g 'co

o

i i i 10 15 20 25 30 35 40 45 Rod Average Burnup (GWD/MTU)

Fig. 7. Fractional Fission Gas Release as a Function of Rod Average Burnup.

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3.10 POST IRRADIATION EXAMINATIONS FOR IASCC STUDY ATJAERI

Takashi TSUKADA, Yukio MIWA, Hirokazu TSUH and Hajime NAKAJIMA

Department of Nuclear Energy System, Tokai Research Establishment Japan Atomic Energy Research Institute Tokai-mura, Naka-gun, Ibaraki-ken, Japan

ABSTRACT

At the Japan Atomic Energy Research Institute (JAERI), a research program on the irra- diation assisted stress corrosion cracking (IASCC) was initiated in 1989. Its objective is to investigate the synergistic effects of high temperature water and neutron radiation on the auste- nitic stainless steel for core internals of both the light water reactors (LWRs) and water-cooled fusion reactor, i.e., the international thermonuclear experimental reactor (ITER). IASCC has been recently recognized as one of the key issues for the integrity of core-internals of aging LWRs including both BWR and PWR. Majorities of experimental data on IASCC have been obtained through the post irradiation examinations (PIEs) such as the slow strain rate testing (SSRT) in high temperature water. This paper presents the outline and requirements for the PIEs conducted for IASCC study.

INTRODUCTION

Core internal materials of the light Fatigue/Creep water reactors (LWRs) such as the austen- Irradiation creep itic stainless steels and Ni-base alloys are Radiation hardening Radiation embrittlement exposed to the high flux neutron/gamma Transmutation reactions radiation and high temperature water en- Swelling, RIS* IASCC vironments. The in-core condition induces Radiation | neutron, y various kinds of material degradation, which are caused by the synergistic effects - Radiation corrosion of the radiation, stress and chemical envi- " (Radiolysis) ' Stress corrosion cracking ronments on the materials. Fig. 1 schemati- Corrosion fatigue cally illustrates the possible degradation of • Hydrogen embrittlement core internal materials. Portions where the 'Corrosion circles are overlapping indicate the syner- RIS*: Radiation induced segregation gistic effects on the materials. As seen in Fig. 1 Schematic illustration of degradation Fig.l, the irradiation assisted stress corro- phenomena experienced by the core materials.

- 325 - JAERI-Conf 99-009 sion cracking (IASCC) can be considered as one of the most complicated degradation phenom- ena suffered by core internals. It is known from the field experiences from LWR plants that IASCC is as an intergranular cracking occurred after an accumulation of neutron fluence be- yond around 5xlO24 n/m2 (E>1 MeV), though the threshold fluence depends on water chemistry and stress level [1-4]. Though the mechanism of IASCC has not been made clear yet, the radia- tion induced segregation (RIS) and subsequent depletion of Cr at grain boundaries is consid- ered to be a major cause of local degradation of corrosion resistance and IASCC. IASCC studies had been started in Japan, Europe and US in the mid 1980s and mainly conducted in relation to the life assessment and extension programs for LWR plants. Recently it is considered that IASCC is one of the most important issues for the plant life management (PLM) of the aged LWRs. This paper gives the outline and perspective of IASCC study at JAERI from a viewpoint of the post irradiation examinations.

HISTORICAL BACKGROUND AND STRATEGY OF JAERI'S IASCC STUDY

At JAERI, studies of the environmentally assisted cracking (EAC) of structural materials, which include the stress corrosion cracking (SCC) and corrosion fatigue (CF), have a root in analyses of the hair-line cracks found in stainless steel overlay lining of the reactor pressure vessel (RPV) of the Japan Power Demonstration Reactor (JPDR) in the late 1960s. For about two decades after the failure in JPDR, EAC studies mainly focused on the corrosion fatigue and subcritical crack growth behavior of low alloy steels, and through this period the test methodol- ogy in high temperature and high pressure water was matured at JAERI. In the late 1980s, officially in 1989, on the basis of the developed methodology, we started an environmental degradation study for core internal materials and it was an initiation of our IASCC study. Fig. 2 shows an overview and flow of IASCC study. For IASCC studies, the post irradia- tion SCC tests, corrosion tests and microscopies are essential techniques. Facilities for these

Core internals In-pile Field experience experiments Failure analyses

IRRADIATION Prediction j^ TECHNOLOGY of degradation^ IASCC Post-irrad. examinations Mechanism Modeling

Unirradiated Alby design material test Plant design Operation guideline

Fig. 2. Flow of IASCC study and applications.

- 326 - JAERI-Conf 99-009 tests had been, therefore, installed at the Oarai and Tokai Hot Laboratories of JAERI. Short descriptions of the facilities and techniques are given in the following sections. In addition to the PEE works, recently efforts are made to develop techniques for in-pile SCC tests to carry out in the Japan Materials Testing Reactor (JMTR), because understanding of simultaneous effect of the radiation, stress and chemical environment on materials is important. Description of in- core experiments is, however, beyond an aim of this paper. As seen in Fig.2, objectives of the IASCC study are to pursue a mechanism of IASCC, to develop counter-measures and to predict material behavior in core of LWRs and other types of reactors. Those activities should be based on the analyses and feedback of field experiences of material degradations in LWRs. We have been carrying out an IASCC study from a viewpoint that this phenomenon is a common issue not only for LWR but also for the advanced reactor systems, e.g., a fusion reactor with water-cooled components. From this view point, three series of PIEs had been performed in JAERFs IASCC study so far. The tested materials are; (1) a type 316 stainless steel irradiated at the Oak Ridge Research Reactor (ORR) under the spectrally tailored irradiation condition to simulate a neutron condition expected on the first wall of the fusion reactor, (2) a cold-worked type 316 stainless steel irradiated at the Japanese experimental fast breeder reactor (FBR) "JOYO" as a wrapper tube of fuel assembly, and (3) the model austenitic stainless steels irradiated at JRR-3M. The materials (1) and (2) were examined to investigate IASCC behavior of materials irradiated under the different neutron condition from that in LWR. The experimental proce- dures and results of PIEs on these three types of materials were reported and discussed else- where[5-12]. In Fig.3, the irradiation conditions of materials used for JAERI's IASCC study are compared. Here, a neutron fluence or dose (dpa) are plotted against a neutron flux or dose rate (dpa/s) because a significant effect of dose rate on radiation damage and IASCC behavior is recently recognized. Irradiation conditions of materials used for our IASCC study are beyond the conditions reported in published IASCC studies and it is the unique point of our study.

Dose of core components JAERI data 60

SI ECIMENS a 2 3

X JRR-3M SPECIMENS IASC^C 107 literature data Dose rate (dpa/s) Fig. 3. Irradiation conditions of materials used for IASCC studies.

327 - JAERI-Conf 99-009

POST IRRADIATION IASCC EXAMINATIONS AT JAERI

1. Slow Strain Rate Testing (SSRT) in high temperature water For IASCC study it is essential to examine a susceptibility to SCC of the irradiated speci- mens in high temperature and high pressure water. There are various kind of SCC test tech- niques that had been developed for the materials used in the ordinary industrial plants. For the post irradiation examinations, SSRT has been most widely applied for IASCC study. SSRT is a tensile test technique with very low constant strain rate in order of 10'7 to 10'5 s1 that causes SCC in a corrosive environment. Fig. 4 shows a flow diagram of the SSRT machine installed in the Oarai Hot Laboratory. SSRT technique has some benefits that are, for example, relatively short testing duration, high sensitivity to SCC susceptibility, controllability of generation rate of slip steps, etc. We had examined, for example, the model austenitic stainless steels irradiated at JRR-3M using the above mentioned test machine. SCC susceptibilities of the irradiated specimens of 14 model alloys were evaluated by SSRT Ar in oxygenated high purity water at 573 Ar+O2 Ion exchanger K. SSRT was carried out at an initial r Hot-cell 7 1 Treatment Monitoring system strain rate of 1.7xlO' s . Electric con- (EO, pH, cond.) ductivities of test water were monitored at inlet and at outlet of the autoclave Autoclave (max. 573K,10MPa) because they are important factor affect- ing SCC behavior. It was maintained below 0.2 (iS/cm at inlet and in a range from 1.0 to 1.7 jiS/cm at outlet. Flow rate of water was controlled at 5 1/h. During SSRT test, the specimens were electrically insulated from the auto- clave. Fracture surface of specimen af- ter SSRT test was analyzed using the scanning electron microscope. Suscep- tibility to SCC was estimated via a frac- Fig. 4. Flow diagram of SSRT machine. tion of the SCC area over the whole 1001 fracture area. This irradiation experi- ment focused on investigating the ef- fects of the minor alloying elements on IASCC behavior. In Fig.5, IASCC sus- ceptibilities of the tested alloys are com- pared and here one can derive the strong effects of additions of C and Mo on IASCC morphology and susceptibility. Detail of the results of PIE were pre- Alloy-ED Fig. 5. IASCC susceptibilities of model stainless sented and discussed in ref.[9,10]. steels irradiated at JRR-3M.

328 - JAERI-Conf 99-009

2. Electrochemical Corrosion Testing A mechanism of IASCC has not been clarified yet, but it can be stated that a local degrada- tion of corrosion resistance of alloys causes an intergranular type SCC, i.e., IASCC, on the irradiated materials. Therefore, corrosion testing after neutron irradiation has the significance not only to pursue IASCC mechanism but also to develop a non-destructive method to assess IASCC susceptibility of alloys. We had chosen electrochemical corrosion test methods for the neutron-irradiated alloys, because these techniques were suitable for PIEs due to the remote acquisition, high sensitivity and short testing time without strong acid. Fig. 6 shows a facility designed for the electrochemical corrosion tests that had been installed in the Tokai Hot Labo- ratory. An irraidated specimen which had mounted in epoxy resin was tested in a electrochemi- cal cell made of acrylic resin where a reference and Pt electrodes were set together. Using this apparatus shown in Fig.6, we carried out the electrochemical potentiokinetic reactivation (EPR) test, potentiodynamic/static measurements, AC impedance tests, and so on.

Test solution a

<0peration area>

Manipulator \ \ Pb glass window Cleaning f*l bath \ Isotheraal water Si

Lock-In asp. Electro- chemical Potentlostat/ cell Galvanostat Electric drain valve

. control unit / Drain tank

Fig. 6. Apparatus for the post irradiation electrochemical corrosion tests.

- 329 JAERI-Conf 99-009

EPR technique was adopted to try to detect Cr depletion due to the radiation induced segregation (RIS). On type 316 alloys, however, it has been noted that modifications of chemi- cal composition of the standard EPR test solution had been always necessary. At JAERI, a modification of standard EPR test method was made for 316 stainless steels irradiated under the spectrally tailored condition and those irradiated in FBRs[7]. EPR tests on the former materials showed slight grain boundary etching only on specimen irradiated at 673 K. As a result, how- ever, it was suggested that for an evaluation of IGSCC susceptibility, the EPR technique was insufficient and the methods to detect both the Cr depletion and impurity segregation, e.g., Coriou tests, may be additionally necessary.

3. Post Irradiation. Microscopies: SEM and TEM analyses After the SSRT tests, all specimens are examined by the scanning electron microscope (SEM) and fractions of SCC are estimated. SEM (JEOL JSM-5400 modified) was installed in a hot cell of the Oarai Hot Laboratory. As an example, SEM photographs of IASCC occurred on the solution-annealed type 316 alloys irradiated up to 8 dpa (2xl026 n/m2) at 673 K and tested in 573 K water[6] are shown in Fig. 7. In this case, the whole area of fracture surface had revealed the intergranular type SCC. RIS of alloy elements at the grain boundaries may be the most important process affecting IASCC. However, since the compositional profiles by RIS in the vicinity to grain boundaries are very narrow around 5 nm in width, qualitative analyses of profiles were only possible by using the conventional type transmission electron microscope (TEM). At JAERI, microstruc- tural analyses of irradiated specimen were performed with a field emission gun type TEM (FEG-TEM, Hitachi HF-2000) installed at the Tokai Hot Laboratory to examine the radiation- induced microstractural and microchemical effects[13,14]. To reduce a detrimental effect of gamma radiation from TEM specimen for the compositional analysis using energy dispersive

Irradiation: 8 dpa <2\ 1026 n/m2) at 673 K in ORR SSRT condition: DO saturated, l.7x107 s"1 at 573 K

• "t

Material: Solution-annealed type 316 stainless steel

Fig. 7. IASCC fracture surface observed by SEM.

- 330 - JAERI-Conf 99-009

spectrometer (EDS), the specimen was miniaturized to 1 mm in diameter. Type 304 model alloys irradiated at JRR-3M were analyzed using the FEG-TEM. Major radiation defects were Frank loops in all alloys and additionally small defect clusters were observed as black dots. No precipitate was found at grain matrix and boundaries in any alloys. Fig.8 shows the microstruc- tures of type 304 alloys; HP3Q4, HP304/C and HP304/SL As shown in Fig.8, addition of C increased the number density of loops, and addition of Si decreased it. These findings are con- sistent with the stress-strain behavior during SSRT of these alloys.

V SI suppressed.

enhanced.

Fig. 8. Microstractures observed by TEM after irradiation at JRR-3M.

4. Other PIE techniques under development for IASCC study at JAERI The above mentioned PIE techniques had been carried out for IASCC study already on the neutron irradiated materials. In addition, other PIE techniques are under development, which are including the crack growth measurement by potential drop technique and surface residual stress analysis by X-ray diffraction technique. These techniques are significant to assess IASCC behavior and PLM of LWR core components because the crack growth data obtained using the former technique and residual stress data obtained using the latter technique will be used to predict the residual life of components in which cracks are detected. At JAERI in the near future, efforts to develop an IASCC crack growth database will be also made.

PIE ISSUES FOR IASCC STUDY

IASCC has been pursued for more than a decade in Asia, Europe and US. However its mechanism has not been satisfactorily understood yet with many unknowns. There are various kinds of technical hurdles to perform IASCC study from a viewpoint of PEE works and many

- 331 - JAERI-Conf 99-009 remaining issues to be solved. However without challenging to overcome the hurdles, there will be no breakthrough to elucidate the mechanism of IASCC. In this section, we summarized and discussed the important issues, which are needed for the future IASCC studies.

1. Advanced testing techniques in high temperature water: 1) High sensitive detection and direct monitoring of IASCC initiation and propagation • Practice of the direct monitoring of crack initiation and propagation is very difficult in high temperature water in the autoclave of testing machine. However, if it is possible, knowledge of IASCC behavior will increase drastically. Potential techniques are, for example, advanced electrochemical techniqe, direct optical observation, etc. 2) Monitoring and control of local water chemistry on specimen under testing • Water chemistry in the autoclave may be different from that of inlet water supplied by the water circulation system. Monitoring and control of chemical condition of high tem- perature water beside the specimen in the autoclave are, therefore, required. For ex- ample, local and micro-volume sampling and analysis techniques are desired. 3) Simulation of in-core radiolysis and/or crevice condition during PIEs • To understand IASCC behavior in the reactor core through PIEs, it is necessary to simu- late the radiolysis of water in core. A technique to inject the hydrogen peroxide into high temperature water is under development. A key issue is an estimation and control of its concentration in the autoclave. 4) Effective IASCC screening test method for irradiated materials • SCC test by SSRT normally takes at least a few weeks and the number of available specimens is limited, so that SSRT is costly in case of PIE. A test technique that can assess IASCC behavior of irradiated alloys for a number of specimens simultaneously in a short duration increases a performance of the PIE. SCC testing using miniaturized specimens is one of the possible techniques.

2. Non-destructive testing techniques: 1) Non-destructive analysis of residual stress inside the irradiated materials • SCC behavior of the materials of plant components strongly depends on the stress condi- tion. An internal stress of the weld portion is especially significant to assess SCC posibility. Neutron diffraction analyses on irradiated materials may enable us to characterize the internal residual stress distribution. 2) Non-destructive evaluation of radiation damage on the irradiated materials • TEM analysis of radiation damage can offer valuable information about microstructural and microchemical conditions, however it is rather destructive analysis and possible only for the miniaturized specimens. Advanced techniques, e.g., electromagnetic method, to detect the radiation damage in a bulk of alloy is desired to be developed.

3. Advanced material characterization techniques: 1) Characterization of oxide film formed on the surface of alloys in high temperature water • To analyze corrosion process through the characterization of specimen surface during

- 332 - JAERI-Conf 99-009

SCC test in the autoclave may be significant to understand the initiation of localized cor- rosion and SCC. 2) Precise analyses of helium/hydrogen in irradiated alloys • Helium produced by nuclear transmutation reaction and hydrogen injected by corrosion process may influence IASCC behavior. Improvements of quantitative analyses of helium and hydrogen contents are imperative to understand these influences. 3) Grain boundary characterization on irradiated alloys • Grain boundary characterization means the analyses of their orientation, morphology, segregation, precipitation, migration, etc. The characterization may be important to under- stand and also to control IASCC propagation process. 4) Detection of the radiation induced segregation (RIS) of alloy elements • To analyze the RIS or depletion of Cr due to RIS, FEG-TEM and Auger microscope are used ordinary, but to perform the microscopies the specimen preparation requires a high level of technique. If advanced techniques, e.g., atomic force microscope (AFM), can be applicable to detect RIS or related microstructure, it will be significantly advantageous.

4. Database for post irradiation IASCC examinations: 1) Development of PIE oriented IASCC database • To analyze the IASCC data from PIEs, various kinds of information such as material, environmental and experimental conditions are required. For the effective data retrieval, the database structures must be suited to the PIE data and IASCC study.

CONCLUDING REMARKS

In 1989, an IASCC study had been officially initiated at JAERI. We have conducted the post irradiation examinations for SCC tests, corrosion test and microscopically analyses and so on. As the mechanism of IASCC has not been clarified at present yet, the post irradiation ex- aminations are essential to pursue the IASCC mechanism and also to develop countermeasures against IASCC. For the further progress of IASCC study, we need to develop/improve the existing PIE techniques and apply the advanced PIE techniques at Hot Laboratories. Since IASCC phenomenon is one of the most complicated processes of materials degradation, IASCC study requires us the interdisciplinary approaches and collaborations in the field of PIE works.

ACKNOWLEDGEMENTS

The authors would like to thanks M. Shindo, S. Kita, S. Jitsukawa, K. Shiba, A. Hisinuma, G.E.C. Bell and T. Kondo for their very helpful supports and discussions. We are also grateful to all staffs of Oarai and Tokai Hot Laboratories for installations of facilities and performing post-irradiation examinations for the IASCC study.

- 333 - JAERI-Conf 99-009

REFERENCES

1. P.L. Andresen, Stress-Corrosion Cracking edited by R.H. Jones (ASM, 1992) p. 181.

2. J.L. Nelson and P.L. Andresen, Proc. 5th Int. Symp. on Environmental Degradation of Mate- rials in Nuclear Power System -Water Reactors (ANS, 1992) p. 10.

3. P. Scott, J. Nucl. Mater. 211(1994)101.

4. T. Tsukada, Proc. 2nd Japan/China Symp. on Materials for Advanced Energy Systems and Fission and Fusion Engineering (1994) p.466.

5. T. Tsukada, K. Shiba, M. Ohmi, et. al., Proc. 3rd Asian Symp. Research Reactor (1991) p.621.

6. T. Tsukada, K. Shiba, G.E.C. Bell and H. Nakajima, CORROSION/92 (NACE, 1992) Paper No. 104.

7. T. Tsukada, S. Jitsukawa, K. Shiba, et al., J. Nucl. Mater. 207 (1993) 159.

8. T. Tsukada and H. Nakajima, J.Nucl. Mater. 212-215 (1994) 1519.

9. T. Tsukada, Y. Miwa and H. Nakajima, Proc. 7th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors (NACE, 1995) p. 1009.

10. T. Tsukada, Y. Miwa, H. Nakajima and T. Kondo, Proc. 8th Int. Symp. on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors (ANS, 1997) p.795.

11. T. Tsukada, Y. Miwa, H. Tsuji and H. Nakajima, J. Nucl. Mater. 258-263 (1998) 1669.

12. T. Tsukada, Y. Miwa, H. Tsuji, et. al., 7th Int. Conf. Nucl. Eng. (ICONE-7) (to be presented)

13. Y. Miwa, T. Tsukada, S. Jitsukawa, et al., J. Nucl. Mater. 233-237(1996) 1393.

14. Y. Miwa, T. Tsukada, H. Tsuji and H. Nakajima, J. Nucl. Mater, (in press)

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3.11 DETERMINATION OF IRRADIATION TEMPERATURE USING SiC TEMPERATURE MONITORS

Tadashi MARUYAMA and Shoji ONOSE

O-arai Engineering Center Japan Nuclear Cycle Development Institute O-arai-machi, Higashi-ibaraki-gun, Ibaraki 311-1393

ABSTRACT

This paper describes a method for detecting the change in length of SiC temperature monitors and a discussion is made on the relationship between irradiation temperature and the recovery in length of SiC temperature monitors. The SiC specimens were irradiated in the experimental fast reactor "JOYO" at the irradiation temperatures around 417 to 645 °C (design temperature). The change in length of irradiated specimens was detected using a dilatometer with SiO2 glass push rod in an infrared image furnace. The temperature at which recovery in macroscopic length begins was obtained from the annealing intersection temperature. The results of measurements indicated that a difference between annealing intersection temperature and the design temperature sometimes reached well over ± 100 °C. A calibration method to obtain accurate irradiation temperature was presented and compared with the design temperature.

INTRODUCTION

The lattice parameter and macroscopic length of neutron-irradiated silicon carbide (SiC) decrease almost linearly with increasing postirradiation isochronal annealing temperature above irradiation temperature. On the basis of this characteristic, SiC has been used as an in- pile uninstrumented irradiation temperature monitor in fast breeder reactors and thermal reactors [1-4]. In the previous studies, the lattice parameter was measured to estimate the irradiation temperature. However, if SiC is irradiated to fluences higher than 1 x 1026 n/m2, the amorphization occurs and due to the line broadening of X-ray diffraction patterns, the lattice parameters are no more determined. Thus SiC monitor is not applicable to the high irradiation region. Bramman [2] and Suzuki et al.[5] measured the dilatation of the irradiated SiC monitors and they pointed out that the onset of recovery was dependent on the heating rate which made it difficult to clearly identify the onset of recovery. Later on, the present author et al. [6] showed a simple method to measure the change in length of SiC temperature monitors by using a differential dilatometer and has shown that the onset of recovery detected

- 335 - JAERI-Conf 99-009 by the step heating dilatometry gives a good agreement with those obtained with an X-ray diffractometer and a micrometer. In regard to the relationship between irradiation temperature and the onset of recovery of SiC which was irradiated in fast reactors, Sharp[7] has reported that the estimated temperature from SiC agreed well with the thermocouple temperature within ± 20 to 25°C. However, Palentine[8] has indicated that there are considerable discrepancies between annealing intersection temperature of SiC and the thermocouple temperature irradiated in the Dounreay Fast Reactor (DFR). He derived the relationship between annealing intersection of specimen length and the irradiation temperature as

Tirrad=1.0312TSiC-44.71 (1) where, Tirrad is the irradiation temperature and TSiC is the annealing intersection temperature obtained by the specimen length measurement. He showed that the accuracy is ± 27 to 45°C. In Japan Nuclear Cycle Development Institute, SiC has been used as one of the off-line temperature monitors to estimate the irradiation temperature of reactor materials. This paper gives the results of measurement of SiC temperature monitor irradiated in "JOYO" experimental fast breeder reactor and the relationship between irradiation temperature and the recovery behavior of SiC temperature monitors is discussed.

EXPERIMENTAL METHOD

The SiC specimens used for the temperature monitor were reaction bonded P-SiC having about 80% of theoretical density and manufactured by Toshiba Ceramics Co. Ltd. The specimens had dimensions typically of 1 mm x 1 mm x 15 mm or 1 mm in diameter and 15 mm long. They were irradiation in the experimental fast reactor "JOYO" to fluences from 0.1 to 63 x 1025 n/m: (E > 0.1 MeV) and the irradiation temperature around 417 to 645 °C (design temperature). The SiC specimens were encapsulated in helium-filled capsules of stainless steel and loaded in the SMIR (Structural Materials Irradiation Rig) and INTA-S (Instrumented Test Assembly - S) irradiation test subassemblies. In SMIR test subassembly, the SiC temperature monitor was irradiated together with a tensile test specimen as shown in Fig. l(a). In INTA-S test subassembly, two kinds of irradiation capsules were prepared. One is called a SMIR- simulated capsule which contains a tensile test specimen and SiC monitor equipped with a thermocouple. This capsule is designed so that it can accurately measure the irradiation temperature of the test specimen and SiC monitor as shown in Fig. l(b). The other capsule is called a temperature monitor test capsule which contains SiC monitor as shown in Fig.l(c). Although it does not provide the thermocouple, the irradiation temperature of SiC monitor could be accurately estimated by taking the thermocouple temperature of SIMR-simulated capsule into account. The design irradiation temperature of SiC monitors in SMIR capsules was calculated from the heat transfer analysis with a universal computer code HEATING-5.

- 336 - JAERI-Conf 99-009

The irradiation temperature of SiC monitors in the temperature monitor test capsule of INTA-S capsules (Fig.l(b)) was calibrated Tensile specimen SiC against the thermocouple temperature in the SMIR-simulated capsule (Fig.l(c)). The change in length of irradiated

specimens was measured as follows: The Fig. 1(a)SMIR capsule length of as-irradiated SiC specimen was first measured by using a conventional micrometer SiC with accuracy of about ±2 |im. Then the specimen was placed in a dilatometer with SiO2 glass push rod in an infrared image 1 furnace and heated up to 900 °C in steps of 50 °C in a nitrogen atmosphere. The temperature Fig. 1 (b) Temperature monitor test capsule was kept for 30 min at each holding temperature. After heating at 900°C, the Tensile specimen SiC Thermocouple specimen was cooled down to room temperature and then the same step heating dilatometry was repeated with the annealed specimen. Taking the difference of dilatation between first and second runs as shown in Fig. Fig. 1(c) SMIR simulated capsule 2, the change in length by annealing of SiC specimen is obtained. The temperature at Fig. 1 Schematic diagram of irradiation which recovery in macroscopic length begins capsules was obtained from the annealing intersection temperature as shown in Fig. 3.

0.00

After anneal recoveiy in o length

o I length change

-0.20 800 1000 annealing temperature (°C) Fig 2 Schematic diagram of step heating Fig. 3 Method for determining irradiation dilatometry temperature of SiC monitors

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RESULTS AND DISCUSSION

Fig. 4 shows the relationship between annealing intersection temperature T and o SMIR siC • p • INTAS the design irradiation temperature Tirrad. It "CD" /• 600 o is shown that the annealing intersection /o 1 I o o o o temperature TsiC is underestimated at o higher irradiation temperature, or s. 500 0 Oo B / overestimated at lower irradiation T3 temperature. Even if we correct the / CO 400 LLJ temperature Tsic by using equation (1) / which was given by Palentine et al., the / 1 1 same tendency still remains and the 300 400 500 600 700 agreement between TSiC and Tirrad was not Design temperature (°C) satisfactory. Fig. 4 Design temperature vs. estimated irradi- We compared the temperature difference ation temperature of SiC monitors obtained between TSiC obtained from annealing from annealing intersection temperature intersection temperature and the irradiation temperature Tirrad as a function of the axial position of SiC monitors in the 160 irradiation subassemblies. As shown in O SMIR Fig. 5, the temperature difference AT, 120 • INTA-S °O v 80 O ° • given as o o 40 0 °

P_ 0 (2) o I pp° < "40 o o is negative around the center region of -80 : ° o reactor core and positive in the bottom or -120 - top region of reactor core. The 4 en -1000 -500 0 500 1000 temperature difference AT sometimes Distance from reactor core center (mm) reached well over +100 °C. In order to find out the cause of the Fig. 5 Difference between design temperature and estimated temperature as a function of large difference between TsiC and Tinad, distance from reactor core center the difference between design temperature and the estimated temperature AT was plotted as a function of neutron fluence. However, the effect of neutron fluence on the temperature difference was not clearly observed. On the other hand, when we plotted the AT as a function of neutron flux, AT is positive when neutron flux is smaller than about 9 x 10" n/(m2 • s) (E > 0.1 MeV) and becomes negative when it is larger than 1x10" n/(m2 • s), as shown in Fig. 6. Palentine [8] has shown that the use of the thermal reactor calibration equation between

Tsic and Tirrid, would lead to serious errors for fast reactor experiments such that the

- 338 - JAERI-Conf 99-009 thermal reactor calibration could cause the temperature in a fast reactor irradiation to be overestimated by up to 23°C at lower temperatures, or underestimate by up to 50°C at higher 160

120 temperature. He pointed out that the e DFR irradiation difference is due to the different dose 80 —D o —•«. rate between thermal and fast reactors. O° O V 40 • O / The dose rate of fast reactor was P about one order of magnitude higher o f V than that of thermal reactor. When Palentine made his investigation of -80 O SMIR X INTA-S SiC monitor in DFR, the neutron flux -120 was in the region of approximately 8 -160 0.5 1 .0 x 10" n/(nr • s) and TSiC was higher 1 .5 9 ! than Timid by about 30°C at about Neutron flux (10' n/m -s) (E>0.1MeV) 560°C. The relationship between AT and the neutron flux given in Fig. 6 yields the AT around 40°C, which Fig. 6 Neutron flux vs. difference in irradiation temperature and the estimated temperature. qualitatively agrees with the correlation eq.(l) given by Palentine. Here, AT is given as = Tsic-Tirra, Thus, it is suggested that SiC monitors which were irradiated in the high flux region resulted in underestimation of irradiation temperature, and those irradiated in lower flux region resulted in overestimation of irradiation temperature. On the other hand, as shown in Fig. 4, the SiC monitors which were irradiated at higher temperature resulted in underestimation of annealing intersection temperatures and those irradiated at lower temperature resulted in over estimation of the annealing intersection temperatures. In the present investigation, the SiC which was irradiated in high flux environment had higher irradiation temperature and low flux at lower irradiation temperature. Since irradiation experiment is not available for the specimens which have been irradiated at high temperature and low flux or at low temperature at high flux, it is difficult to clearly indicate that the onset of recovery in length of SiC is influenced by the neutron flux or the irradiation temperature. Furthermore, in the present investigation, the most of design irradiation temperature is based on the heat transfer calculation which sometimes brings about ambiguity as to the accuracy of irradiation temperature and makes it difficult to compare the irradiation temperature and the temperature derived from SiC monitors. Therefore, in determining irradiation temperature of SiC monitors, it is necessary that the SiC temperature should be directly measured with thermocouples. We consider that further systematic investigation is needed to elucidate effect of neutron flux and/or irradiation temperature on the recovery behavior of SiC temperature monitors.

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SUMMARY AND CONCLUSION

In the present investigation, the change in length of SiC temperature monitors was measured by a step heating dilatometry. The temperature at which recovery in macroscopic length begins was obtained from annealing intersection temperature and we obtained the following results and conclusion. (l)The results of measurements indicated that a difference between annealing intersection temperature and the design temperature sometimes reached well over ± 100 CC. (2) Higher irradiation temperature resulted in lower annealing intersection temperature of SiC monitors and vise versa. (3) It was suggested that the onset of recovery of SiC is influenced either by the neutron flux or the irradiation temperature. (4) Since the specimens were available only for those irradiated at high temperature and high flux or low temperature and low flux, the origin of the difference is not clear at present. (5) Systematic irradiation experiment is needed to elucidate the cause of difference between irradiation temperature and that obtained from SiC monitors, where, the temperature of SiC monitors should be directly measured with thermocouples.

REFERENCES

1. N. F. Pravdyuk, V. A. Nikolaenko, V. I. Karpuchin and V. N. Kuznetsov, Properties of Reactor Materials and the Effect of Radiation Damage, proceedings ed. by D.J. Litter, Butterworths, London (1962) 57. 2. J. I. Bramman, A.S. Fraser and W.H. martin, J. Nucl. Energy, 25(1971) 223. 3. R. J. Price, Nucl. Technol., 16 (1972) 536. 4. J.E. Palentine, J. Nucl. Mater., 61(1976)243. 5. H. Suzuki, T. Iseki and M. Ito J. Nucl. Mater., 48(1973)247. 6. T. Yano, K. Sasaki, T. Maruyama et al., Nucl. Technol.,93 (1991)412. 7. R. M. Sharpe, British Nucl. Ener. Soc, London (1980) 71 8. J.E. Palentine, J. Nucl. Mater., 92(1980)43.

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3.12 R&D STATUS AND REQUIREMENTS FOR PIE IN THE FIELDS OF THE HTGR FUEL AND THE INNOVATIVE BASIC RESEARCH ON HIGH-TEMPERATURE ENGINEERING

Kazuhiro SAWA1, Masahiro ISHIHARA2, Tsutomu TOBITA1, Junya SUMITA1, Kimio HAYASHI2, Taiji HOSfflYA3, Hajime SEKINO4, Etsurou OOEDA4

Department of HTTR Project1 Department of Advanced Nuclear Heat Technology2 Department of JMTR3 Oarai Research Establishment Japan Atomic Energy Research Institute Oarai-machi, Higashiibaraki-gun, Ibaraki-ken, Japan Department of Hot laboratories4 Tokai Research Establishment Japan Atomic Energy Research Institute Tokai-mura, Naka-gun, Ibaraki-ken, Japan

ABSTRACT

The High Temperature Engineering Test Reactor (HTTR), which is the first high temperature gas-cooled reactor (HTGR) in Japan, achieved its first criticality in November 1998 at the Oarai Research Establishment of the Japan Atomic Energy Research Institute (JAERI). In the field of HTGR fuel development, JAERI will proceed research and development (R&D) works by the following steps: STEP-1) confirmation of irradiation performance of the first-loading fuel of the HTTR, STEP-2) study on irradiation performance

341 - JAERI-Conf 99-009 of high bumup SiC-coated fuel particle and STEP-3) development of ZrC-coated fuel particle. Requirements for post-irradiation examination (PIE) are different for each R&D step. In STEP-1, firstly, hot cells will be prepared in the HTTR reactor building to handle spent fuels. In parallel, general equipments such as those for deconsolidation of fuel compacts and for handling coated fuel particles will be installed in the Hot Laboratory at Oarai. In STEP-2, precise PIE techniques, for example, Raman spectroscopy for measurement of stress on irradiated SiC layer, will be investigated. In STEP-3, new PIE techniques should be developed to investigate irradiation behavior of ZrC-coated particle. In the field of the innovative basic research on high-temperature engineering, some preliminary tests have been made on the research areas of 1) new materials development, 2) fusion technology, 3) radiation chemistry and 4) high-temperature in-core instrumentation. Requirements for PIE are under investigation, in particular in the field of the new materials development. Besides more general apparatuses including transmission electron microscopy (TEM), some special apparatuses such as an electron spin resonance (ESR) spectrometer, a specific resistance/Hall coefficient measuring system and a differential scanning calorimeter (DSC) are planned to install in the Hot Laboratory at Oarai. Acquisition of advanced knowledge on the irradiation behavior is expected in these two HTTR-related fields through close cooperation between the user and hot laboratory groups of JAERI including the present authors.

INTRODUCTION

The High Temperature Engineering Test Reactor (HTTR)[1,2] is a test reactor with a thermal output of 30MW and outlet coolant temperatures of 850 and 950°C at the rated operation and the high temperature test operation, respectively. This reactor uses the pin-in- block type fuel, and has capability to demonstrate nuclear process heat utilization. An overview of the HTTR facility is shown in Fig. 1, and major specifications of the HTTR are listed in Table 1. Construction of the HTTR was started in March 1991, and the first criticality was achieved on November 10, 1998. The research and development (R&D) using the HTTR is scheduled in a wide range 1) to establish the technology basis on high temperature gas-cooled reactors (HTGRs), 2) to

- 342 - JAERI-Conf 99-009 upgrade present HTGR technologies, 3) to establish high-temperature nuclear process application technologies and 4) to make the innovative basic research on high-temperature engineering. R&D of HTGR fuel is carried out to establish the technology basis on HTGRs and to upgrade the present HTGR technologies. The innovative basic research is carried out to explore innovative high-temperature technologies using irradiation facilities. In the field of HTGR fuel, JAERI will proceed R&D works by the following steps: STEP-1) confirmation of irradiation performance of the first-loading fuel of the HTTR, STEP-2) study on irradiation performance of high burnup SiC-coated fuel particle, and STEP- 3) development of ZrC-coated fuel particle. In the field of the innovative basic research on high-temperature engineering, some preliminary tests have been made on the research areas of 1) new materials development, 2) fusion technology, 3) radiation chemistry, and 4) high-temperature in-core instrumentation. This report describes present status of R&D and requirements for PIE in the field of the HTGR fuel development and the innovative basic research on high-temperature engineering.

POST IRRADIATION EXAMINATION PROGRAMS FOR HTGR FUEL

1. Characteristics of HTGR fuel In HTGRs, coated fuel particles are employed as fuel to permit high outlet coolant temperature. In current high temperature gas-cooled reactors (HTGRs), Tri-isotropic (TRISO)-coated fuel particles are employed as fuel. The TRISO coatings consist of a low- density, porous pyrolytic carbon (PyC) buffer layer adjacent to the spherical fuel kernel, followed by an isotropic PyC layer (inner PyC; IPyC), a silicon carbide (SiC) layer and a final PyC (outer PyC; OPyC) layer as shown in Fig. 2. In a safety design of the HTGR fuels, it is important to retain fission products within particles so that their release to the primary coolant does not exceed an acceptable level. From this point of view, the basic design criteria for the fuel are to minimize the failure fraction of as-fabricated fuel coating layers and to prevent significant additional fuel failures during operation [3]. The future R&D concerning the HTGR development is scheduled in a wide range mainly using the HTTR. The R&D subjects, which aim at improving the performance and economy

- 343 - JAERI-Conf 99-009 of HTGR, are concerned mainly with the advancement of basic HTGR technologies and improvement of the core performance. As for coated fuel particles, it is important to improve fission product retention capability of the fuel with a high power density and a high burnup durability under long-term high temperature operation [4]. A modified SiC-TRISO coated fuel particle is selected as a high burnup fuel. In order to achieve higher burnups up to 10%FIMA, thickness of the buffer and SiC layers is increased in the design. At the same time, the kernel diameter is somewhat reduced to mitigate the internal pressure in a coated fuel particle increased by the higher burnup. Furthermore, HTGR fuels in the next generation are required for higher temperature utilization and an enhanced safety. For the higher temperature utilization of the HTGR fuels, a key issue is adoption of a new coating material, which is more refractory than SiC used in the conventional coated fuel particles. Since zirconium carbide (ZrC) is one of the promising materials to meet this requirement, development works on the ZrC coating have been conducted at JAERI. The works are going to be upgraded in an engineering scale including production, property and irradiation studies. On the background described above, JAERI will proceed R&D works in the field of HTGR fuel by the following steps: STEP-1) confirmation of irradiation performance of the first-loading fuel of the HTTR, STEP-2) study on irradiation performance of high burnup SiC-coated fuel particle and STEP-3) development of ZrC-coated fuel particle. Requirements for post-irradiation examination (PIE) are different for each R&D step. Table 2 summarizes major PIE items and apparatuses required for each R&D step.

2. PIE of the first-loading fuel of the HTTR The PIE of the first-loading fuel of the HTTR is carried out to confirm its irradiation performance and to obtain data on its irradiation characteristics in the core. Hot cells will be prepared in the HTTR reactor building to handle spent fuels. In parallel, general equipments such as those for consolidation of fuel compacts and for handling of coated fuel particles will be installed in the Hot Laboratory of the JMTR. The first-loading-fuel of the HTTR assembly is so-called a pin-in-block type of hexagonal graphite block containing fuel rods as shown in Fig. 3. A fuel rod consists of a graphite sleeve and of 14 fuel compacts. In a fuel compact, about 13,000 TRISO coated fuel particles are dispersed densely in the graphite matrix made from graphite powder and phenol

344 - JAERI-Conf 99-009 binder. The kernel of the coated fuel particle is low-enriched (average 6wt%) UO2, 600 urn in diameter. The fuel rods are inserted into bore holes in a hexagonal graphite block. Helium coolant flows through the annular gaps between the fuel rods and the boreholes. Fuel handling and storage systems in the HTTR are shown in Fig. 4. The maximum burnup is designed to be 33 GWd/t as a block average value. After about three years operation, the fuel assemblies are transferred to the spent fuel storage pool in the reactor building by the fuel handling machine. The irradiated fuel assembly is disassembled to the fuel rods and a graphite block in the HTTR cell. Then the fuel rods are transferred to the Hot Laboratory of the Japan Materials Testing Reactor (JMTR) at JAERI Oarai, by a cask for the PIE. In the Hot Laboratory, failure fractions, burnup, etc. are inspected as shown in Table 2. In the safety design of HTGR fuel, it is important to retain fission products within the coated fuel particles so that their release to the primary coolant may not exceed an acceptable level. Since fission products are almost completely retained by the coating layers, the dominant sources of fission product release are failed particles and contaminated uranium in the fuel compact matrix[5]. The through-coatings failed particle and uranium contaminated uranium in the fuel compact matrix determine the fission gas concentration in the primary coolant during operation. From this point of view, the free uranium fraction is one of the most important PIE items. On the other hand, since the as-fabricated SiC-failed particle does not have the mechanically strongest coating layer, SiC, the as-fabricated SiC-failed particle is predicted to result in the through-coatings failed particle by internal pressure during operation. The intact particle is predicted not to fail in the HTTR operating condition [6], It means that the as-fabricated SiC-failure fraction determines the additional through-coatings failure fraction, i.e., increase in fission gas concentration in the primary coolant during operation. From this point of view, as-fabricated failure fraction is important. The free uranium fractions of the fuel compacts were measured by the electrochemical deconsolidation followed by the acid leaching [7]. The SiC-failure fractions of the fuel compacts were measured by the burn/leach method [7]. Figure 5 shows the flows of fuel failure fraction measurements.

During the HTTR operation, the fuel behavior is monitored by fission gas concentration in the primary coolant, which is continuously measured by three ionization chambers. The

- 345 - JAERI-Conf 99-009 signals are used to initiate a reactor scram under abnormal operating conditions. When the fission gas concentration is increased up to a value corresponding to the 0.2% failure, the location of failed fuel is detected by fuel failure detection (FFD) system. The FFD system detects the failure of coated fuel particles by measuring gamma rays from condensable fission products precipitated on the wire. Finally, post-irradiation heating, which corresponds to the shipping test for the LWR fuel, should identify failed fuels. We are developing a post- irradiation heating method for a fuel rod and an analytical method to quantify the failure fraction by measuring the activity of 85Kr released from a heated fuel rod.

3. PIE of high burnup SiC-coated fuel particle The target burnup and fast neutron fluence of the high burnup SiC-coated fuel particle are higher than those of the first-loading fuel of the HTTR [8]. In order to keep the fuel integrity up to high burnups over 5%FIMA (% fission per initial metallic atom), thickness of the buffer and SiC layers of the fuel particle has been increased in the specification. The configuration of the high burnup SiC-coated fuel particle is summarized in Table 3, comparing with the first-loading fuel of the HTTR. In order to confirm the integrity of the high burnup SiC-coated fuel particle, behavior of the coating layer should be investigated. PIE techniques required for the investigation of the high burnup SiC-coated particle are basically the same as those for the first-loading fuel, except handling of the high burnup fuel. The major PIE items are measurements of the burnup and the through-coatings and SiC-layer failure fractions. In addition, we are trying to develop a technique to measure the stress in the SiC layer by, for example, the Raman spectroscopy or the X-ray diffraction analysis. The obtained stress data will be used to understand the quantitative relationship between the internal pressure and the coating failure and to develop an improved fuel failure evaluation code.

4. PIE ofZrC-coatedfuel particle Major characteristics of the ZrC-coated fuel particle are its high temperature resistance (much higher than 1600°C which is the criteria for SiC-coated particle) and weakness against oxidation [9,10]. Considering these characteristics, R&D should be carried out concentrating on ZrC behavior at high burnups and high temperatures, and on its oxidation

- 346 - JAERI-Conf 99-009 behavior. In development of ZrC-coated fuel particle, new PIE techniques should be devised to investigate its irradiation behavior. Since a ZrC layer is easily oxidized by burning, the burn-leach method can not be applicable to measurement of the failure fraction of ZrC-coated particle, while this method is useful for the SiC-coated particle, . Therefore, an alternative method to measure the failure fraction should be developed. In this respect, a plasma oxidation technique was developed in order to remove the OPyC layer of unirradiated ZrC- coated particle [11]. We will investigate applicability of this method to irradiated ZrC- coated particle.

R&D STATUS AND PIE PLANS FOR THE INNOVATIVE BASIC RESEARCH PROGRAM ON HIGH-TEMPERATURE ENGINEERING

/. Outline and scope of the innovative basic research program The innovative basic research concerns with basic science and technology which are associated with high-temperature radiation environments [1,12]. The research directions involve novel challenges both in nuclear and non-nuclear fields. At the beginning of the program, more than sixty themes were proposed in a wide variety of research fields such as new materials development, fusion technology, radiation chemistry, high temperature in-core instrumentation. Through discussions, a total of eight subjects have been selected for preliminary tests using out-of-pile facilities and currently available irradiation facilities, in order to examine and demonstrate their scientific and technical feasibility and effectiveness in envisaged HTTR irradiation.

2. Irradiation facilities of HTTR Irradiation facilities of HTTR, which are available for the innovative basic research program, was described elsewhere in detail [13]. In brief, four kinds of irradiation regions are available for irradiation, as shown in Fig. 6 [1,14]. Two types of special irradiation capsules were preliminary designed so far; one is a rotation drive type capsule [15], RDC, and the other is an irradiation creep capsule.

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A recent investigation on requirements from the new materials development has revealed, however, that an irradiation device with a simpler structure than the RDC would be more appropriate for early stage works, which still aim at searching and confirming optimum irradiation conditions to develop the high-temperature SiC semiconductors and high critical- temperature (Tc) superconductors. Any type of the HTTR capsules, however, will surely produce a large amount of irradiated samples to be tested mainly in the JMTR Hot Laboratory.

3. Preliminary irradiation tests and PIE plans An outline of preliminary tests of eight on-going research subjects is listed in Table 4 [12]. The present status of the preliminary tests and the plans for the envisage HTTR irradiation are described below [14], together with PIE plans which are associated with the preliminary irradiation using other reactors and with the real HTTR irradiation. An investigation on the PIE plans and apparatuses have been made by a committee of the Atomic Energy Society of Japan including some of the present authors, on the new materials development, which are in a technical level deserving concrete investigations.

3.1 Neutron transmutation doping (NTD) of high temperature semiconductor Silicon carbide (SiC) has recently been received attention in its application to high- temperature, high-power and high-speed switching devices. Conventional diffusion techniques to introduce impurities are not applicable to this material, because SiC is not readily permeable to impurity elements. In stead, phosphorus (P) ion implantation using accelerators and neutron transmutation doping (NTD) of P using reactor thermal neutrons are regarded as promising. The latter is the most suitable to large samples, because of its essential capability to form completely homogeneous distribution of dopant elements. In a view of preliminary NTD experiments, thin expitaxial films of 3C-SiC (cubic in crystalline structure) and 6H-SiC (hexagonal) were irradiated with N+, P+ and A1+ ions at temperatures up to 1200°C and annealed at temperatures between 1000 and 1600^. The irradiated samples were characterized by the electron spin resonance (ESR) and the Hall effect measurement for the residual defect-spin density and electrical activation. Figure 7 shows the defect spin density, which was measured by ESR as a function the implantation temperature, for p-type 6H-SiC samples irradiated with 200keV P+ ions [16]. This figure

- 348 - JAERI-Conf 99-009 indicates that defects generated during implantation are annealed out with increasing the implantation temperature up to 1200^. The ESR spectrometer and the Hall effect device should be essential in the PIE of neutron irradiated samples. These apparatuses are expected to be installed in a hot experimental room. In addition to them, it is necessary to facilitate an annealing furnace which can anneal irradiated samples at least up to 1600t. A set of these equipments in a small scale should be installed already in an early stage of the preliminary neutron-irradiation experiments. This is because the PIE data obtained from the specimens are going to be utilized for specifying the most appropriate condition of the real HTTR irradiation. In this respect, a recent preliminary irradiation test by a JMTR capsule (97M-13A) indicated that some of the irradiated samples are considerably radioactive due to impurity activation. This result implies that they cannot be taken out of a hot (radioactive) area to a cold (non-radioactive), at least for a while after irradiation. The best place for PIE to obtain the data quickly after irradiation will be a hot experimental room where the irradiated samples can be treated without heavy radiation shielding .

3.2 Irradiation processing of high-Tc superconductor It has recently been revealed that when an oxide superconductor with a high critical temperature (Tc) is irradiated with high-energy neutrons or heavy ions, the induced lattice defects clusters act as traps of external magnetic fluxes which are going to invade the superconductor and to lead to degradation of the superconductivity. This irradiation processing technique is feasible in increasing the critical current density (Jc), which is one of the key parameters for the practical use of oxide high-Tc superconductors. In realizing this technique, the use of HTTR with a large irradiation space is suitable to large ingot samples, which can be used as large super conducting magnets. The R&D status for this work is somewhat immature, compared with that for the NTD study described above. The optimum conditions of the neutron fluence and the irradiation temperature have been pursued by post-irradiation annealing in the preliminary irradiation experiments. Figure 8 is a typical example, in which the critical current density (Jc) of Bi-

2212 (Bi2Sr2CaCu20x) superconductor samples have increased by more than two orders of

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22 2 magnitude by fast neutron irradiation to a fluence of 5x10 n/m (E>lMeV) with subsequent annealing at 400°C for one day [17]. Apparatuses for this radiation processing research on superconductors, such as a superconducting quantum interference device (SQUID), are not generally used in PIE of other conventional ceramic and metallic materials. A concrete investigation on the installation of the apparatuses will be made after obtaining relevant data, such as whole activity and its decay tendency of radioactive nuclides produced in irradiated samples.

3.3Research on radiation damage in ceramic composite materials Advanced structural materials for very high temperature components have been directed to particulate or fiber reinforced composite materials. For nuclear applications, carbon/carbon (C/C) and silicon carbide/silicon carbide (SiC/SiC) composites have been considered most favorable in plasma facing components as well as in HTGR control rod elements. Engineering properties of any fiber- or particulate-reinforced ceramic composite material are known to be controlled by reinforcing material grade, volume fraction, weaving or forming, interface and matrix properties. In addition, these controlling factors changes in a very complicated manner under high-temperature neutron irradiation environment [12]. Following a proposal made by Arai [18], a series of basic-oriented studies has been started in 1997 on radiation damage/effects of typical ceramic composites. Some candidates tentatively selected for the preliminary out-of-pile and irradiation tests are listed in Table 5. The first irradiation was successfully completed in December 1998 in a temperature range of 3OO-55O°C by a JMTR capsule designated 97M-13A. The specimens have just been subjected to PIE. A preliminary measurement of radioactivity revealed that some specimens are rather highly activated, which implies that main facilities for PIE should be prepared in hot cells, and not in hot experiment rooms. The second and the third irradiation experiments will be performed at temperature ranges of 600-900°C and 1000-1200°C in 1999 and 2000, respectively. PIE items under planning are i) dimensional change, ii) thermomechanical properties such as thermal expansivity and creep parameters, m) thermal properties such as thermal diffusivity and specific heat capacity, iv) mechanical properties such as bending strength,

- 350 - JAERl-Conf 99-009 and others. These measurements are rather general for ceramic materials, but the absolute values and the anisotropy of these properties are significantly different from those for monolithic materials. More general apparatuses such as a transmission electron microscope (TEM) and an image analyzer of microstructures, e.g. pore size distribution, are needed in an early stage. Furthermore, special consideration on the methods and apparatus designs for PIE is needed, following the progress in the PIE works for the preliminary irradiation tests. An example is a differential scanning calorimetry (DSC) system for measuring the specific heat capacity, which is to be altered for PIE. These kinds of works are being proceeded intensively and extensively through close cooperation between user and hot laboratory groups of JAERI including the present authors.

SUMMARY

The HTTR aims at establishing and upgrading the HTGR technology basis, and will be used as a tool for the innovative basic research on high-temperature engineering. In the field of HTGR fuel, JAERI will proceed R&D works by the following steps: STEP-1) confirmation of irradiation performance of the first-loading fuel of the HTTR, STEP-2) study on irradiation performance of high burnup SiC-coated fuel particle and STEP- 3) development of ZrC-coated fuel particle. The requirements for post-irradiation examination (PIE) are different for each R&D step. (1) The PIE of the first-loading fuel of the HTTR is carried out to confirm its irradiation performance and to obtain data on the irradiation characteristics in the core. Hot cells will be prepared in the HTTR reactor building to handle the spent fuels. In parallel, general equipments such as those for deconsolidation of fuel compacts and for handling of coated fuel particles will be installed in the Hot Laboratory of the JMTR. (2) The major PIE items for the study on irradiation performance of high burnup SiC-coated fuel particle are measurements of burnup and failure fractions. In addition, we are trying to develop the SiC stress measurement technique by, for example, Raman spectroscopy and X-ray diffraction analysis. (3) For development of ZrC-coated fuel particle, new PIE techniques should be developed to

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investigate its irradiation behavior. R&D should be carried out concentrating on ZrC behavior at high burnups and high temperatures, and on the oxidation characteristics. In particular, the method to measure the failure fraction should be developed.

In addition, the present R&D status was briefly described for the innovative basic research on high temperature engineering. The PIE plans and apparatuses are being investigated in the field of the new materials development. (1) In the NTD research for the high-temperature SiC semiconductor, examinations are being made on installation of a set of special apparatuses for ESR and the specific resistance/Hall effect measurement, together with the post-irradiation annealing furnace. (2) As for the researches on high-temperature super-conducting materials and ceramic composite materials, tentative plans are made to install some general apparatuses such as TEM and the image analyzer. Concrete plans to install special apparatuses, such as SQUID, are being made steadily, following the progress in the PIE works for the preliminary irradiation tests.

ACKNOWLEDGEMENTS

The present authors are deeply indebted to JAERI members in relevance, in particular, to Dr. T. Tanaka, Mr. H. Mogi and Mr. T. Kikuchi of the Department of HTTR Project, Dr. Y. Miyamoto and Dr. S. Shiozawa of the Department of Advanced Nuclear Heat Technology, Dr. O. Baba of the Department of JMTR and Dr. T. Kodaira of the Department of Hot Laboratories, for their cooperation and encouragement. Thanks are also due to Dr. T. Arai of Office of Planning of JAERI, to members of universities and JAERI who are in collaboration with some of the present authors on the innovative basic research, and to the Special Committee of the Atomic Energy Society of Japan and the HTTR Utilization Committee of JAERI both headed by Prof. S. Shiori, for their cooperation and support for the research.

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REFERENCES

1. Japan Atomic Energy Research Institute, Present Status of R&D of HTGR Research and Development (1997) (in Japanese). 2. S.Saito, T.Tanaka, Y.Sudo, O.Baba, et. al., JAERI-1332 (1994). 3. K.Hayashi, S.Shiozawa, K.Sawa, S.Sato, et al., JAERI-M 89-161 (1989). 4. S.Shiozawa, K.Sawa, K.Fukuda and N.Kitamura, Proc. IAEA TCM, Petten, Netherlands, Nov. 28-29, 1995, p.290. 5. K.Sawa, S.Shiozawa, K.Fukuda and Y.Ichihashi, J. Nucl. Sci. Technol., 29, 1992, p.842. 6. K.Sawa, S.Shiozawa, K.Minato and K.Fukuda, J. Nucl. Sci. Technol., 33, 1996, p.712. 7. F.Kobayashi, S.Shiozawa, K.Hayashi, K.Sawa et al., JAERI-M 92-079 (1992). 8. K.Sawa, S.Yoshimuta, JAERI-Tech98-025 (1998). 9. T.Ogawa, K.Fukuda, S.Kashimura, T.Tobita, et al., J. Am. Ceram. Soc, 75, 1992, p.2985. 10. K.Minato and K.Fukuda, Proc. IAEA TCM, Beijing, China, 1995, p.86. 11. T.Ogawa and K.Fukuda, Surface Modification Technologies, 1990, p.309. 12. T. Arai, H. Itoh, T. Terai and S. Ishino, Proc. OECD/NEA/NSC Workshop on High Temperature Engineering Research Facilities and Experiments, Nov. 12-14, 1997, Petten, The Netherlands; ECN-R-98-005 (1998), p. 113. 13. K. Sanokawa, T. Fujishiro, T. Arai, Y Miyamoto, T. Tanaka and S. Shiozawa, ibid., p.145. 14. T. Kikuchi, Japanese Patent Toku-Kai-Hei 9-222493 (1997). 15. Japan Atomic Energy Research Institute, Present Status of High Temperature Engineering Research (in Japanese), 1999. 16. K.Abe, T.Ohshima, H.Itoh, YAoki. M.Yoshikawa. I.Nishiyama and M.Iwami, Proc. Int. Conf. on Silicon Carbide HI, held in Stockholm, Sweden, August 31-September 5, 1997. 17. T.Terai, T.Kobayashi and YItoh, Sci. Rep. RITU A45 (1997) p. 15. 18. T. Arai, Proc. 2nd IEA Workshop on SiC/SiC Composites for Fusion Structural Applications, Sendai, Japan, October 23-24, 1997.

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Table 1 Major specification of the HTTR. Thermal power 30 MW Outlet coolant temperature 850/950 °C Fuel Low enriched UO2, Prismatic block Heat removal IHX and PWC (parallel loaded) Primary coolant pressure 4MPa Containment type Steel containment Plant lifetime 20 years

Table 2 Major items and required apparatus for PIE of HTGR fuel. Items Apparatus First-loading • Disassemble of fuel rod • Hot cell in HTTR reactor building fuel of the • Fuel rod handling device HTTR • Disassemble of fuel compact • Cutter, etc. * Dimension measurement • Linear scale, etc. • Failure fraction measurement • Coated particle handling device • Electrolytic disintegration device • Burnup measurement • Ge-detector • X-ray radiography • X-ray radiograph • Ceramography • Polisher • Optical Microscope • Non-destructive failure • Sweep gas furnace for fuel rod fraction measurement High burnup • Capsule disassembling • Grinder, etc. SiC-coated • Micro structure analysis of • Scanning Electron Microscope (SEM) fuel SiC layer • Transmission Electron Microscope (TEM) • X-ray diffractometer • Raman spectroscopy • Fission product release • Sweep gas furnace for fuel compact and measurement coated fuel particle ZrC-coated • Failure fraction measurement • Plasma oxidation apparatus fuel • Oxidization test • Furnace of air and water vapor injection

Table 3 Comparison of high burnup fuel and the first-loading fuel of the HTTR. High burnup fuel First-loading fuel Maximum burnup (GWd/t) 50-100 33 Fast neutron fluence (1025m'2) 3-5 1.5 Kernel diameter (um) 550 600 Buffer layer thickness (um) 90 60 SiC layer thickness (um) 35 28-30

- 354 - Table 4 Summary of the present preliminary tests.

Research Field and Title Experimentals methods Measurements New Materials Development • high temperature SiC semiconductor • sample: SiC single and polycrystals • residual defects by ESR by neutron transmutation doping • hot-implantations of P* in TIARA and annealing • electron concentration • thermal neutron irradiations in JMTR (Hall coefficient) • Improvement of high-Tc superconductor • sample: Bi-2212 single crystal • critical current density and by neutron irradiation • fast neutron irradiations in JMTR and post- irrreversibility field at irradiation annealing 4.3K-60K > Machanistic radiation damage studies • samples: SiC/SiC and C/C composites etc • microstructural.features by on ceramic-based structural composites with/without pre-heat treatments XRD, SEM, TEM • fast neutron irradiations in JMTR •CTE en 2 High Temperature Radiation Chemistry O CO Ol o O1 • Radiation enhanced thermal decomposition of • sample: silicon-containing polymers and PAN • product mass spectrum by 3 polymers • gamma-ray irradiations above 400°C EPR spectrometry O • Irradiation-assisted precursors curing for O SiC fiber and carbon fiber Fusion Material/Component

• Mesurement of physicochemical properties of • samples: LJO2, Li+SiO+ • contact potential difference lithium oxides under irradiation • performance tests in out-of-pliles and in YAYOI and electrical conductivity High Temperature Reactor Instrumentation • Development of a heat amd radiation resitant • preparation of large core diameter silica fibers • optical transmissivity by optical fiber system • out-of pile high temperature endurance tests optical power meter and • performance tests under irradiation in JMTR spectrum analyzer • Development of ceramic-based neutron/gamma • sensor: polycrystalline BN • electrical current induced detectors including SPNDs ' performance tests under irradiation in KUR by high temp., neutron flux and gamma-ray Table 5 Candidate test materials for carbon- and silicon carbide-based composites.

Material system Candidate test material Carbon fiber Fiber • PAN-derived reinforcing • Coal tar pitch-derived Carbon system • Petroleum pitch-derived Continuous fiber reinforced C/C composite • (not favored) Short fiber reinforced C/C composites > ffl • 2D-felt 2 I • Sheet o CO Particulate • Graphite containing large seeds reinforcing © o Polygranular • Isotropic graphite(reference) • HOPG Silicon carbide Fiber PCS-derived fiber system reinforcing • NICALON™ • HI-NICALON™ Continuous fiber reinforced SiC/SiC composite - CVI-SiC/SiC(HI-NICALON™) Particulate • a-SiC containing large seed particles reinforcing • a -SiC containing platelets JAERI-Conf 99-009

Air cooler

Refueling machine

Reactor pressure vessel

Intermediate heat exchanger

Pressurized water Reactor cooler containment vessel

Fig. 1 HTTR facility.

t.iQ, kernel Buffer layer PyC

SIC Inycr

Fig. 2 The TRISO-coated fuel particle.

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Fuel handling hole Fuel kernel Dowel pin Plug High density PyC SiC Fuel Low density PyC ^compact 6.92mm Graphite 'sleeve 8 mm

39mm

34mm

Fig. 3 First-loading-fuel of the HTTR.

Maintenance pit Ceiling crane

Fuel handling machine New fuel storage cell Refueling hatch

Irradiated materials storage pit

HTTR fuel handling cell

Reactor containment vessel Spent fuel storage pool Reactor pressure vessel

Fig. 4 Fuel handling and storage systems in the HTTR.

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|Fuel compact

[Electrolytic disintegration!

|Coated fuel particle

JHNO-, leaching

[Colorimetric analysis]

Measurement of exposed uranium fraction

[Fuel compact]

[Burning

Burn-back SiC-particle

HNO, leaching

[Colorimetric analysis!

Measurement of SiC-failure fraction

Fig. 5 Flow of fuel failure fraction measurements.

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©Replaceable reflector region A (3 columns) ©Test fuel loading region (3 columns)

©Center column region (1 column)

©Replaceable reflector region B (12columns) ©Permanent reflector region (4 holes)

Fig. 6 Irradiation positions in the HTTR. (Regions ®@(D(5) are available for materials irradiation.)

0 200 400 600 800 10001200 Implantation Temperature (°C) Fig. 7 Dependence of residual defect spin density on implantation temperature for 6H-SiC samples implanted with 200keV-P+ ions to lxl0i5/cm2.

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1010 : Fluence:5X1018(n/cm2) Irradiation temp.; Room temperature Measuring temp.; 40 K Anneal tempVAnneal time 4001 Alday

5 £ 10 Without anneal treatment

0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 Magnetic field (T)

Fig. 8 Changes in critical current density (Jc) due to neutron irradiation and subsequent thermal annealing. (Irradiation at low temperatures to 5xl018n/cm2 and post-irradiation annealing at 400 and 800 °C.)

- 361 - JAERI-Conf 99-009 JP9950654

3.13 ADVANCED POST IRRADIATION EXAMINATION FOR FUSION REACTOR DEVELOPMENT IN JMTR

Kunihiko TSUCHIYA, Etsuo ISHITSUKA, Minoru UDA, Junichi SATTO and Hiroshi KAWAMURA

Department of JMTR, Oarai Research Establishment Japan Atomic Energy Research Institute Oarai-machi, Higashi-ibaraki-gun, Ibaraki-ken, Japan

ABSTRACT

The evaluation on function of fusion reactor components, i.e. blanket, plasma facing components (divertor, etc.) and vacuum vessel used under the neutron irradiation is indispensable in order to design fusion reactor components in detail. Therefore, three kinds of new facilities shown as follows are established in JMTR hot laboratory. Outlines of these new facilities and advanced data examined with these new facilities are explained in this paper.

INTRODUCTION

The evaluation on function of fusion reactor components, i.e. blanket materials, plasma facing components (divertor, etc.) and vacuum vessel used under the neutron irradiation, is indispensable in order to design fusion reactor components in detail. Therefore, three kinds of new facilities shown as follows are established in JMTR hot laboratory and these facilities are used for post irradiation examination (PIE). From now, outlines of these new facilities are explained in turn. In this paper, outlines of these new facilities and advanced PIE data with these new facilities are described.

Fig. 1 Three new facilities in hot laboratory in JMTR.

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NEW FACILITY FOR NEUTRON MULTIPLIER

Beryllium is expected to be used as a neutron multiplier and plasma facing material in fusion reactor. Then, beryllium irradiation studies were performed with Japan Materials Testing Reactor (JMTR) to get the engineering data for fusion blanket design. New facility for the post irradiation examination of neutron-irradiated beryllium was constructed in the hot laboratory of JMTR [1]. This facility named "Beryllium PIE facility", consists of the five glove boxes, dry air supplier, tritium monitoring and removal system, storage box of neutron-irradiated samples. Maximum amount of tritium handling in the facility is 7.4 GBq/d (200 mCi/d). Ventilation system of the beryllium PIE facility is shown in Fig. 2. Tritium release apparatus, laser flush apparatus for thermal property measurements and mechanical test apparatus have already been installed in glove box No. 1 (GB-1), No.4 (GB-4) and No. 5 (GB-5), respectively. An apparatus of reprocessing will be installed in glove box No.2/3 (GB-2/3) in near future. Each apparatus in glove boxes is summarized in Table 1.

Storage box Exhaust Ttritium process monitor blower

_t V2 GB-5 GB-1 GB-2/3 GB-4 Dry air supplier

V3 V4 GB: Glove box V : Changing valve of normal and Tritium removal tritium removal mode system GB-1 : Tritium release properties GB-2/3: Reprocessing properties GB-4 : Thermal properties GB-5 : Mechanical properties Fig. 2 Ventilation system of beryllium PEE facility.

Table 1 Outline of each apparatus in glove boxes Items Test Test condition Remarks temperature Tritium release R.T.~ Helium sweep Measurement of gaseous tritiated properties 1300°C gas or vacuum water and tritium gas Thermal R.T.- Vacuum Measurement of thermal properties 1200 °C 2.7xlO-5 Pa diffusivity and heat capacity at700°C Mechanical R.T.~ Vacuum Tensile test, Bending test properties 800 °C 2.7xl0"3Pa Compression test at 800 °C

- 363 JAERI-Conf 99-009

/. Tritium release properties Tritium release properties from neutron-irradiated beryllium that have different grain size, have been studied. Specimens were beryllium produced by the hot-press method (specimen name :BHP, grade :S-65C, grain size :0.01mm) and the vacuum casting method (specimen name :BVC, grade :B-26D, grain size :0.56mm). These specimens were cut from the bending test specimen [2]. Each beryllium specimens were irradiated by JMTR with a He production rate of about 0.3 and l.OxlO3 appm and irradiation temperature of about 327°C and 616°C in helium, respectively. From the SEM observation of fractured surface after bending test, it has been already clear that helium bubbles exist on the grain boundaries in high temperature irradiated specimens. From tritium release experiment, following results were observed [2]. For the larger-grained specimens, apparent diffusion coefficient was larger than that of the small-grained specimens, and did not change by the effect of helium bubbles on the grain boundaries. Result for the small-grained specimens is shown in Fig. 3. A double peak was observed on heating BHP (irradiation condition : O.3xlO3 appm, 327°C) at 900°C. Apparent diffusion coefficient of the second peak was two orders larger than that of the first peak. Helium bubbles on the grain boundaries acted as trap sites at low temperature and accelerated the tritium release by the bubble connection at high temperature.

1500 200 BHP .2nd peak

cc p 150 c

2 .a 2 100 E CD K ca | 500 50 2 1st peak 'E 0 3000 4000 5000 6000 Time (s) Fig. 3 Double peak of tritium release curve.

2. Thermal properties Beryllium disk specimens (^lOxtl.4 mm, grain size: 0.02 mm, purity : 99.3%) irradiated with a total fast neutron fluence of 4.5xlO20 n/cm2 (E>1 MeV) at about 200°C were measured by the laser flash method to study the thermal properties of neutron irradiated beryllium [3]. The specimens swelled by the annealing up to 1200°C after irradiation were also measured by the laser flash method. Thermal conductivity of the beryllium disk specimens decreased to about 90% of the original value by neutron irradiation. This decrease was presumably caused by the neutron irradiation defects. Furthermore, for the annealed specimens with AV/V(swelling rate)=0.29 and

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AV/V=0.63, it decreased to about 70% and 40% of that of the un-irradiated specimen, respectively. These decreases of the thermal conductivities seemed to result from the decrease of density and the heat insulation effect of helium cavities generated in the annealed specimen [3]. Thermal conductivity as a function of swelling rate (AV/V) is shown in Fig. 4. Effect of swelling can be estimated by using the equation of Meredith [3]. By using the swelling estimation calculation code (for example ANFIBE code) and the equation of Meredith, it is possible to predict the thermal conductivity of neutron irradiated beryllium at high temperature, and also to predict the thermal diffusivity by calculation because specific heat is not changed by neutron irradiation and swelling. Effect of irradiation defects and/or helium production on thermal conductivity seems smaller than that of effects of density decreasing. However, more detailed study will be necessary to understand the thermal properties. Additionally, thermal expansion coefficients should be measured for the design conditions of fusion blanket.

Temp. l.inirrariiatfic IrraHiatar .2.0 19 "C o • • • •;flrvr. A \K'\Nv [ : Meredith

1.0 8 0.5 -I . CD

i • i • 0 0 0.2 0.4 0.6 0.8 Swellinarate (AV/V) Fig. 4 Thermal conductivity of beryllium specimens as a function of swelling.

3. Mechanical properties The fracture stress for beryllium bending specimens (4x3x40 mm) produced by the BHP and BVC method was measured by the mechanical test apparatus. Irradiation conditions of the beryllium bending specimens were shown in Table 2.

Table 2 Neutron irradiation condition. Inner capsule Ti.r Neutron Fluence (E > lMeV) No. (°C) (n/cm2) 1 327 1.3X102' 2 445 3.0x1021 3 616 4.3x1021 4 524 4.1x1021

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Fracture stress of beryllium bending specimens as a function of irradiated temperature is shown in Fig. 5. The decrease of the fracture stress was observed at high temperature irradiated for BHP specimen (irradiation condition : 4.3xlO21 n/cm2, 616°C, AV/V=O.O33). However, decreasing of the fracture stress was not observed in BVC specimens (AV/V=0.011), although the irradiation conditions are the same as those for BHP specimen. Helium bubbles were observed on grain boundaries. Decrease of the fracture stress was presumably caused by helium bubbles on grain boundaries, because fracture mechanism changed from intergranular fracture for the specimens irradiated at low temperature to intergranular fracture for the specimens irradiated at high temperature. It was obvious that these fracture stress of irradiated specimens was dependent on the grain size. From now, impurities and other effects also must be studied in details.

Unirradiated

800*

700

S. 600

500

400 £ BHP (grain size: 0.01mm) 2 300 BVC (grain size; 0.56mm) "- 200

100

0 0 100 200 300 400 500 60 70 Irradiated temperature ('(X) 0 Fig. 5. Fracture stress of beryllium bending specimens as a function of irradiated temperature.

ELECTRON BEAM FACILITY FOR PLASMA FACING COMPONENTS R&D

Plasma facing materials and components such as the first wall and the divertor of the fusion reactor (ITER) will be exposed to high heat loads and high neutron flux generated by the plasma. Based on this reason, many high heat flux tests for un-irradiated materials and water cooled mock-ups have been reported [5-6]. However, there are a little studies of the neutron irradiation effect for the performance of these materials and the components during the high heat flux test. Therefore, the high heat flux tests of neutron irradiated specimens have been performed using Oarai Hot-cell electron Beam Irradiating System (OHBIS) which was installed in a hot cell of a hot laboratory of the Japan Materials Testing Reactor (JMTR) [7]. OHBIS consists of the electron beam unit and the vacuum vessel that is placed under the electron beam unit. As main performances of OHBIS [7], the maximum power of the electron beam is 50kW, and the heating period is more than 0. lms. And, the acceleration voltage and the maximum beam current of the electron beam unit are 30kV (constant) and 1.7A,

- 366 JAERI-Conf 99-009 respectively. It is estimated that OHBIS can produce a heat flux as high as 2.5 GW/m2 that is calculated value at (|)5mm of the electron beam. By the way, carbon fiber reinforced carbon composites (CFCs) are one of candidate materials for the plasma facing components. However, the neutron irradiation effect for the erosion behavior of CFCs during thermal shock test has not been studied. These studies are indispensable for the design of the plasma facing component, because the thermal conductivity of CFCs decreases by the neutron irradiation [8]. Therefore, the thermal shock tests of neutron irradiated CFC specimens were performed using OHBIS. Tested specimens are 1-directional type CFCs (MFC-1), 2-directional felt type CFCs (CX2002U) and 3-directional type CFCs (NIC-01). The dimension of the specimens is 'll.5xwllxh7.5 mm. These specimens were irradiated with the total neutron fluence of 0.3- 0.4dpa at 283-321°C using the JMTR. The un-irradiated and irradiated specimens were tested in the present test campaign. As the heat load condition by electron beam, two kinds of conditions were selected to investigate the effect of different heat fluxes, i.e. 500 MW/m x40ms and 800 MW/m x25ms on bombardment damages. The active cooling for the specimen was not used. The thermal shock tests were performed in vacuum (8xl0~3 Pa). Weight losses of specimens on MFC-1 and CX2002U are shown in Fig. 6 as a function of neutron fluence for different heat fluxes. The weight loss increased almost linearly with neutron fluence, and is about two times larger than that of the un-irradiated specimens. The weight loss of CX2002U is larger than that of MFC-1. The maximum depth of the erosion was not changed with neutron irradiation. Increase of the weight loss was presumably caused by degradation of thermal conductivity because of neutron irradiation [9].

Heat flux Materials (MW'nr2) MFC-1 CX2002U 4 -- 500 A 800 • 3 - o I A o 2 - ISO « 8 -

1 1 1 1 0 0 0.1 0.2 0.3 0.4 0.5 Neutron fluence / dpa Fig. 6 Weight loss of CFCs to neutron fluence.

Figure 7 shows the erosion profiles for different neutron fluences for MFC-1 and CX2002U. It can be seen that the area and the full width at half maximum (FWHM) of the erosion increase with neutron fluence. Increase of spot at FWHM is presumably caused by degradation of thermal conductivity and damage of neutron irradiation on the structure between carbon atoms due to neutron irradiation. The surface morphology of the specimens is shown in Fig. 8. It is observed that erosion area of the CFCs increased with neutron fluence [9-10].

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Un-irradiated

Neutron Fluence 0.4 dpa

CX2002U Un-irradiated i ^J^ 0.4 dpa CO 1 \ I -3 -2 -1 0 1 Position / mm Fig. 7 Typical erosion plofiles of MFC-1 and CX2002U (Heat flux : 500MW/m2)

Fluence / dpa Materials 0

MFC-1 (1-D)

CX2002U ( 2-D) ' -'•' .'.•""' '•

NIC-01 I" •*'" ~ ? ^ 10 mm (3-D)

Fig. 8 Surface morphologies of samples tested under the disruption conditions (500MW/m2x40ms).

As a result of the surface morphology in MFC-1 after the neutron irradiation observed by scanning electron microscope, it is observed that some cracks were initiated at heated area, and fiber and matrix were uniformly eroded. In CX2002U after the neutron irradiation, it is observed that the carbon fibers and matrix were preferentially evaporated and that the impregnated materials which had originally covered the fibers were remained. This tendency is the same as the un-irradiated samples [5].

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RE-WELDABILITY TEST FACILITY FOR VACUUM VESSEL R&D

Rewelding of irradiated materials has large impact on the design and the maintenance scheme of in-vessel components. Recently, joining technology with irradiated structural materials, such as stainless steels and inconel alloys, has been investigated in the way of tungsten inert gas (TIG) welding, laser welding and so on [11-12]. However, helium is one of the most prominent transmutation products generated in these materials because of the high cross section for (n, a) nuclear reactions of high energy neutrons of fusion reaction [13]. And helium is essentially insoluble in metals. The generation of helium is known to degrade the properties of materials. The formation of grain boundary (GB) bubbles can ultimately lead to drastic changes in microscopic properties , including severe embrittlement at elevated temperature. At high temperature, these bubbles will grow under the influence of stress and temperature [14-15]. Welding processes produce internal stresses and elevated temperatures. Joining performances with irradiated materials have been reported in the previous paper [16]. However, systematic evaluation of weldments have not been performed in the previous papers. Performances of remote controlled welding machine and milling machine are shown in Table 3 and Table 4, respectively. These apparatus were equipped in the concrete cells at the JMTR (to see Fig. 1). Flow chart of reweldability test is shown in Fig. 9. The specimens irradiated in JMTR were welded by the TIG welding method. After welding, welding specimens were processed by the milling machine and mechanical properties of weldments were performed. In the present time, weldments of un-irradiated and/or irradiated materials (type 316 stainless steel and Inconel 625) were performed by the TIG welding method, and mechanical properties of their weldments were systematically evaluated [16-17]. Effect of irradiation on tensile strength of weldments of Inconel 625 is described as follows. Tensile strengths of un-irradiated/un-irradiated weldment (Weld A) and irradiated/un-irradiated weldment (Weld B) were 850 MPa and 866 MPa at 20°C, respectively, and these strengths were almost similar to that of the un-irradiated base metal. Weldments of Weld A and Weld B fractured at the part of the un-irradiated base metal.

Table 3 Performance of remote controlled welding machine. Input Power Voltage 100V Line Current 20A/100V Welding Range 1-100A Output Power Peak Pulse 100A Voltage 40V Moving Range (Stage) X axis : 50 mm Remarks Y axis : 50 mm Least Command Increment 0.01 mm Maximum Gas Flow Rate 8000 cnrVmin

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Table 4 Performance of remote controlled milling machine. Milling System Cooling System Control of Milling Machine Gearbox of Main shaft Air Capacity Axis 1000 - 3000 rpm 500 cm3/min Triaxial concurrency control Moving Range Air Pressure Control unit Work table (X axis) 1 - 5 kg/cm2 0.001 mm 280mm Air Temperature Automatic operation Cutting (Y axis) -40°C Automatic start 250 mm Automatic feed Work head (Z axis) Automatic stop 150 mm Manual operation Crashing Speed Step feed 5 - 500 mm/min Rapid traverse Least Command Increment 0.001 mm

Fabrication of specimens

Neutron irradiation

Rewelding by remote control

Fabrication of tensile specimens

Post Irradiation Examination (PIE) - Tensile test - Hardness test - Metallographical observation - SEM, XMA Fig. 9 Flow chart of reweldability test.

Effect of irradiation on tensile strength of weldments of Inconel 625 at 150°C is shown in Fig. 10. Tensile strengths of weldments of Weld A and Weld B were 796 MPa and 802 MPa at 150°C, respectively, and these strengths were similar to that of the un-irradiated base metal, because weldments of Weld A and Weld B fractured at the part of the un-irradiated base metal. On the other hand, tensile strength of irradiated/irradiated weldment (Weld C) were 560 MPa and 813 MPa at 20°C and 150°C, respectively, and these strengths were smaller than that of the irradiated base metal at each temperature, because weldments of Weld C fractured at the part of the weld metal or heat affect zone (HAZ). Especially, tensile strength of Weld C was smaller than that of the un-irradiated base metal at 20°C, and this reason will be evaluated by the other tests, i.e. hardness tests, SEM observation, etc. SEM micrographs of fracture surfaces of three combinations of weldments after tensile testing were observed. Main fracture of these specimens was ductility. SEM micrographs of cross section for the irradiated/un-irradiated weldment (Weld B) is shown in Fig. 11. The small bubbles were observed at the parts of weld

- 370 - JAERI-Conf 99-009 metal and HAZ on the irradiated side. The size of these bubbles was approximately 0.5 |im. The bubble size observed in this study was similar to the bubble size obtained in the reweldability test with SS316 irradiated under the same irradiation condition. It was considered that helium bubbles have grown at grain boundary under high temperature and internal stress, which occurred during the welding process. From the results of this tests, data on several characterization of reweldability by TIG welding method will be obtained for the design potential of fusion reactor.

1000 TestTemp.:150°C WelcH WeldB 800 _ - I / \

Q. 600 i\ Weld A -s—» f/x C 400 V 36 X Weld A: un-irr./un-irr. 200 Weld B: irr./un-irr. Weld C: irr./irr. 0 i i i 0i 20 40 60 80 Strain (%) Fig. 10 Effect of irradiation on tensile strength of weldments of Inconel 625 at 150°C.

r '>!,,— j ! I

I I

Fig. 11 SEM micrographs of cross section for the irradiated/un-irradiated weldment (Weld B).

SUMMARY

It is urgent to obtain various engineering data for detail design of fusion reactor such as HER and DEMO reactor. At present, PIE on blanket materials, plasma facing components (divertor, etc.) and vacuum vessel have be performed with these facilities which have been equipped in

- 371 - JAERI-Conf 99-009

JMTR and data on several characterization will be obtained for the design potential of fusion reactor.

ACKNOWLEDGMENTS

We would like to acknowledge the support of the hot laboratory stuffs of the JMTR for the post irradiation examinations (PIEs).

REFERENCES

1. E.Ishitsuka and H.Kawamura, CONF-9509218 INEL (1995)269-278. 2. E.Ishitsuka, H.Kawamura, T.Terai and S.Tanaka, Fusion Technology (20th-SOFT), Volume 2(1998)1281-1284. 3. E.Ishitsuka, H.Kawamura, T.Terai and S.Tanaka, Fusion Technology (19th-SOFT), Volume 2( 1996) 1503-1506. 4. E.Ishitsuka, H.Kawamura, T.Terai and S.Tanaka, J. Nucl. Mater., 258-263(1998)566- 570. 5. M.Araki, M.Akiba, M.Seki, M.Dairaku, H.Ise, S.Yamazaki, S.Tanaka and K.Yokoyama, Fusion Eng. Des., 19(1992)101-109. 6. M.Akiba, M.Araki, K.Nakamura, S.Sato, S.Suzuki, M.Dairaku, K.Yokoyama and Y.Ohara, Fusion Technology (19th-SOFT), Volume 1(1996)307-310. 7. S.Shimakawa, N.Sakamoto, K.Satoh, M.Akiba and H.Kawamura, J. Nucl. Mater., 233- 237(1996)1582-1585. 8. T.Maruyama and M.Harayama, J. Nucl. Mater., 195(1992)44-50. 9. M.Uda, E.Ishitsuka, K.Sato, M.Akiba, C.Yamamura, S.Takebayashi and H.Kawamura, Fusion Technology (20th-SOFT), Volume 1(1998)161-164. 10. M.Uda, E.Ishitsuka, K.Sato, M.Akiba, C.Yamamura and H.Kawamura, 8th international workshop on Carbon Materials, to be published in Physica scripta. 11. M.M.Hall, Proc. 5th Bolton Landing Conf., Aug. 1978, General Electric Co., Schenectary, NY (1979). 12. E.V.van Osch, ECN-RX-94-074 (1994). 13. H.R. Brager and J.L.Straalsund, J.Nucl. Mater., 46(1973)134-158, 14. H.T.Lin, M.L.Grossbeck andB.A.Chin, Metallurgical Transactions A, 21A( 1990)2585- 2596. 15. C.A.Wang, H.T.Lin, M.L.Grossbeck andB.A.Chin, J. Nucl. Mater., 191-194(1992)696- 700. 16. K.Tsuchiya, H.Kawamura and R.Oyamada., J. Nucl. Mater., 233-236(1996)218-223. 17. K.Tsuchiya, N.Sekimura, F.Matsuda, G.Kalinin, M.Shimizu and H.Kawamura, Fusion Technology (20th-SOFT), Volume 2(1998)1297-1300.

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3.14 HOT CELL WORKS AND RELATED IRRADIATION TESTS IN FISSION REACTOR FOR DEVELOPMENT OF NEW MATERIALS FOR NUCLEAR APPLICATION

Tatsuo SHIKAMA

Oarai Branch, Institute for Materials Research, Tohoku University Oarai, Ibarakiken, 311-1313 Japan Telephone,29-267-4947, Facsimile;29-267-4947, e-mail; [email protected] ac.jp

ABSTRACT

Present status of research works in Oarai Branch, Institute for Materials Resarch, Tohoku University, utilizing Japan Materials Testing Reactor and related hot cells will be described.Topics are mainly related with nuclear materials studies, excluding fissile materials, which is mainly aiming for development of materials for advanced nuclear systems such as a nuclear fusion reactor. Conflict between traditional and routined procedures and new demands will be described and future perspective is discussed.

INTRODUCTION

Hot cells will handle mainly irradiated nuclear-fission-fuels and materials. Nowadays, hot cells handling irradiated fuels are strictly discriminated from those handling non-fissile materials only. Irradiated fuels and trans-uranium elements are very dangerous and strict regulations and well-equipped hardware are needed there. These situations have not changed since the beginning of development of fission nuclear systems. Rather, the regulations and needed hardware tend to become more and more strict as our knowledge concerning these so-called alpha-emitters increases. In the meantime, it is clear that situations surrounding hot cells and hot cell works handling non-fissile materials are changing rapidly. One example will be related with material researches for advanced nuclear system in long-term prospects, where majority of Japanese university researchers are working. In this paper, hot cells and hot cell works handling non-fissile materials will be discussed. Material researches utilizing fission reactors and hot cells have now a long history since 1940s[l,2,3,4]. In some senses, they have been enjoying well-established technologies and procedures, which have been developed in the 1940s and early 1950s in nuclear-advanced countries[5]. They were a part of a so-called large-scale science and technology whose major

373 - JAERI-Conf 99-009 parts were related with military purposes, spending much expenditure and consuming a lot of men-powers and material-resources. It means that they have been executed with a well-organized long-term plan, in other words it means being not flexible to unexpected changes of situations. Still, major parts of works related with fission reactors and hot cells have residues reflecting such a preceding history. Some people still claim that inflexibility and a rigid-framework with a long-term-plan are mainly related with securing safety-issues which will be essential for nuclear systems. However, rational and detailed analyses of present procedures will reveal that major parts of present strict procedures will not have essential relation with today's safety. Rather, it can be said that they come from the automatic adoption of historically-developed procedures in nuclear advanced countries, whose major parts are not always relevant to the nowadays works. When late-comers are trying to catch up with advanced outriders, adoption of established procedures will be the most efficient way. However, when we try to go ahead without any guiding models, we have to reconsider total systems and we have to construct our original ways. Material researches utilizing fission reactors and hot cells in Japan as well as in Korea will be in that situation now.

PRESENT SITUATIONS

In the past history of nuclear developments, a major role of hot cells would have been a handling of spent fuels, being highly radioactive especially with alpha-emitting trans-uranium elements. There, rigid and stubborn procedures were needed to secure safety and to satisfy safeguard for non-proliferation of fissile materials. A major part of present hot-cell regulations and hot-cell software/hardware were apparently established to correspond to these situations. In our present situations, many hot-cells are being used for developing new materials, which are not fissile nor alpha emitters, for advanced nuclear systems. Also, our systems have strict discrimination between so-called alpha-cells (hot cells handling alpha emitters and materials contaminated with alpha-emitters) and so-called beta-gamma cells (hot cells handling materials non-fissile and emitting only beta- and gamma-rays). Thus, our beta-gamma cells are usually free from alpha contamination, being contrast to hot cells in nuclear advanced countries, where alpha contamination should be always worried about, even in cells presently used for handling only beta-gamma emitting materials. In the course of early developments of nuclear fission systems in nuclear advanced countries, well-selected materials have been irradiation tested. Testing items were deliberately decided and executed following a long-term strategy. At the same time, a majority of irradiation tests were simple ones using no-instrumented rigs or at the best instrumented with a few thermocouples. In-situ type irradiation tests such as creep tests were rigorously carried out only by the early 70s, mainly for special demands from such as military purposes. In the meantime, we have to handle a variety of candidate materials, from conventional metallic materials to advanced materials and material systems such as less-common-metals, ceramics, ceramic-fiber-composites and semiconductors. There, frequent and speedy iterations

- 374 - JAERI-Conf 99-009 are needed, among development of materials, materials irradiation in fission reactors and post irradiation examinations (PIEs) of irradiated materials in hot cells. Especially, as advances of new materials are very fast in contemporary industries, irradiated materials and material systems will become out-of-data and PIEs will be useless, if we have to wait for PIEs for a extended period after irradiation. Also, a variety of tests are demanded now, from conventional tests such as simple mechanical tests using standard-size specimens and microstrutural examinations by conventional optical and electrical microscopes, to mechanical tests using miniaturized specimens such as a nano indenting test, and analyses by advanced electrical systems, such as a field-emission analytical electron microscope (FEAEM) and a scanning tunnel microscope (STM). Also, demands for examination of functional properties such as thermal conductivity and electrical properties are increasing. Another example of new demands for hot cell works will be heat-load tests and welding tests for heavily irradiated materials. Finally, complicated irradiation techniques in fission reactors are demanded for developments of advanced nuclear materials. Examples will be re-irradiation of irradiated and radio-activated materials, iteration of irradiation among different reactors, such as between a fast-reactor which have hard neutron spectrum and a thermal reactor which has a mixed neutron spectrum. Isotope tailored irradiation, namely, materials containing designed amount of isotopes to simulate nuclear transmutation, is becoming popular especially for developments of nuclear fusion materials. There, radioactive and expensive isotopes may sometimes have to be handled in hot cells. And, more fully-equipped installations in radiation capsules (rigs) are demanded for measuring irradiation conditions properly. Recent studies are revealing that an irradiation temperature is very important parameter for radiation effects in materials. Temperature measurements are the most fundamental monitor for any scientific experiments. However, accumulated results in fission reactor irradiation are revealing that temperature measurements were not sometimes accurate enough to understand observed radiation effects. Also, variation of temperatures among specimens in one radiation capsule sometimes turned out far larger than that expected by thermal analysis before irradiation. We should be cautious about temperatures measured by non-grounded sheathed thermocouples, especially when we study temperature-transient effects. Figure 1 shows comparison of temperatures measured by conventional K-type non-grounded sheathed thermocouple with those measured by optical fibers, in Japan Materials Testing Reactor (JMTR) in Oarai Research Establishment of Japan Atomic Energy Research Institute [6]. In the case of measurements by optical fibers, intensity of black-body-radiation from sapphire

(single crystal alumina(Al2O3) was measured using fused silica (SiOi) core optical fibers. The optical fibers used in this measurement were radiation-resistant and its optical transmission does not degrade by the irradiation in the concerned optical wavelength, namely in the range of 1000-1800nm [7]. Good agreements between results obtained by the thermocouple and the optical measurements at steady state irradiation for a extended irradiation period supports this. The temperatures measured by the optical measurements showed extensive overshoot at the beginning of irradiation, in the meantime, overshoot of the temperatures measured by the

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800 100 Thermocouple — Optical fiber • 700 80 FT Vi l^tuwwim*—*^ 600 * • 60 |

atur e [ ( r " o Q. 500 40 o CO Tempe r CD 400 20 *

i * i 0 50 100 150 200 250 300 Irradiation time [h]

Figure 1 Temperature measured by optical fiber in comparison with that mesured by thermocouple in JMTR. thermocouple is small. Deviation in two measurements was about 20K at the most. Some experiments are suggesting that the deviation of temperatures measured by non-grounded sheathed thermocouples from real temperatures may exceed 100K. In many cases, engineers handling radiation capsules tend to prefer using fatter thermocouples for easier handling and for more reliable performance especially at higher temperatures. Also, present regulation usually forbid using grounded and open-type thermocouples in radiation capsules. However, now we have many and long-period experiences using mineral insulated cables (Mi-cables) and thermocouples in fission reactors and it will not necessarily jeopardize safety if we use fine and open-type thermocouples, which will improve accuracy of temperature measurements substantially. And, occasionally, in-situ measurements are needed on once irradiated materials. Here, complicated and delicate hot-cell works are essential to handle radiation capsules(rigs) with radioactive contents. There, disassembling and re-assembling of radioactive systems of delicate

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EfG 96-6116

HFIR HORIZONTAL-V- MID-PLANE

CAPSULE FACILITY TUBE

Fig. 2. Axial cross-section of the irradiation capsule.

- 377 - JAERI-Conf 99-009 structures with many cables have to be carried out in hot cells. The works will need welding, soldering of irradiated materials. Also, they have to handle many of fine thermocouples and Mi-cables. Figure 2 shows schematic structures of radiation capsule used for measurements of electrical conductivity of ceramic insulators under irradiation in High Flux Isotope Reactor (HFIR) in Oak Ridge National Laboratory (ORNL) under US/Japan collaboration called JUPITER project [8,9]. Fifteen specimens were accommodated and 15 triaxial and coaxial Mi-cables and 33 thermocouples had to be handled. Now, the capsule was disassembled and electrical conductivity of each specimen is under measurements in a hot cell in ORNL successfully.

PROSPECTS OF FUTURE HOT-CELL RELATED WORKS FOR MATERIALS RESEARCH

Above described demands to hot cell works are not always compatible with historically developed strict procedures for hot cell works nor with detailed structures of hardware of present hot cells. Thus, some new ideas for hot cell works are urgently needed not only in procedures but also in hardware. Several attempts have been made to have newly designed hot cells for developments of nuclear fusion materials using high-flux fusion-neutron sources, such as International Fusion Materials Irradiation Facility (IFMIF). However, it looks that most of their attempts were still strongly influenced by historical constraint. It will be a good idea to have internationally organized workshops for stimulating fresh and free-from-historical-constraint to have newly designed hot cells. Currently developed modular-type hot cells will be one example for new-type hardware satisfying new demands. Here, it should be noted that the modular-type hot cells were developed for demands from works handling alpha-emitters. However, this kind of new ideas can be extended to accommodate above-mentioned new demands. New hot cells should allow us easy access to dismantle and re-install test equipments. They also should have potential to allow us to handle large number of small specimens and sometimes to allow us quasi-contact access to specimens for delicate and complicated handling. At the same time, reevaluation of software for utilizing various kinds of hot cells available now is important. One example will be a relationship between well-equipped hot cells in JAERI and small but convenient hot cells in university open facility of Oarai Branch of Tohoku University. JAERI's hot cells are operated under a long-term plan, thus they have little flexibility to ad-hoc demands. Also, they are in general very expensive to operate, admitting that they are well-equipped and their operators have high-level skills and that their safety-guarantee is above standard. They will be good at handling a large irradiated fixture and carrying out standardized and large-demands tests such as a standard tensile test. In the meantime, small-cells will have advantage in corresponding to temporary demands and to tailored and detailed works. Mutual collaboration will be one of the first steps for establishing new structure of future hot-cell works. Also, international collaboration will become very important. As hot-cell related works

- 378 - JAERI-Conf 99-009 are very resource-consuming, one country can not have self-fulfilled total systems. The collaboration between the USA and Japan on nuclear fusion materials, which is called as JUPITER (Japan/Usa Program on Irradiation Test using Reactors) program, will give us one example. General hot-cell works are done in large-scale hot cells in the USA after materials were irradiated in fission reactors in the USA. After that, depending on what is demanded for further experimental works, specimens were delivered to research institutes in Japan as well as in the USA, where they have small hot-cells equipped with special research tools. Collaboration between Korea and Japan on hot-cell works is strongly anticipated.

References

1.R.G.Hewlett, O.E.Anderson, F.Duncan, A History of the United States Atomic Energy Commission, Vol. I, Vol. II, Vol. Ill, (1990) University of California Press, California. 2. M.Gowing, Britin and Atomic Energy, (1964) Independent and Deterrence I, II, (1974) Macmillan, London. 3. V.C.Jones, United States Army in World War II, Special Studies, Manhattan: The army and the atomic bomb, (1985) U.S.Army Center of Military History, Washington D.C.. 4. T.Rockwell, The Rickover Effect, (1992) United States Naval Institute, Annapolis, Maryland. 5. K.G.Benefiel edited, The Plutonium Story, (1994) Battelle Memorial Institute< Columbus Ohio. 6. F.Jensen, T.Kakuta, T.Shikama, T.Sagawa, M.Narui, M.Nakazawa, Fusion Eng. Design, 42(1998)449. 7. T.Shikama, T.Kakuta, M.Narui, T.Sagawa, J. Nucl. Mater., 253 (1998) 180. 8. S.J.Zinkle, T.Shikama et al., DOE/ER-0313/20 (1996) 257, -0313/22 (1997) 179, 188, 9. T.Shikama, S.J.Zinkle, et al., J. Nucl. Mater., 258-263 (1998) 1861, 1867.

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Summarizing Talk by Norikazu Ooka Deputy director, Department of JMTR

It's great pleasure for me to summarize special through this seminar on PIE technologies. The time is coming close so that I'd like to summarize briefly and quickly The first session, as the recent activities of KAERI, JAERI, JNC, NFD, NDC, Tohoku Univ. and Hanyang Univ. , the overview of facilities were introduced by 9 presenters. As regarding the elementary technique such as TEM, crack measurement, SEM, small punch testing and NDT using ultrasonic were also presented by 5 speakers. For the utilization technique such as reassembling, electric discharge cutting and welding were introduced by 3 speakers. Otherwise, for the evaluation of PIE data, we will be able to make three categories, that is the core internals, life time evaluation and driver fuels. Totally 9 presentations on the behavior of core internals, control rod for ECT , cladding tube / RCCA for PWR rod cluster control assemblies, and life time evaluation for RPV such as charpy impact test, tensile test and microanalysis, and Zr-2.5Nb of fracture toughness and so on, and also the behavior of driver fuel for research reactor and PWR, and also Hydride failure, FP gas release, burn up were given by the expression. Final session give us the very important information to regarding the IASCC, analyzing irradiation temperature, advanced PIE for HTTR & fusion and PIE and related irradiation test to future around the research and development of PIEs. In this final session, from the view point of scientific and technical research, user's requirement and newly PIE techniques were proposed. I think, it will be recommended the close correlation between in-situ and post-irradiation experiments and international mutual collaboration, especially JAERI-KAERI and related facilities in Japan are indispensable and should be established in order to make an important roll to get the break through in the field of nuclear power and to promote PIE activities to the next step. I believe that, we have learned a lot from this seminar and have got successful results. I would, therefore, like to thank participants, especially Prof. T. Shikama of TOHOKU Univ. and Prof. Y-S. Kim of Hangyang Univ., our guest speaker from Tokai hot laboratories, JNC, NFD, NDC and related institute, and also Dr. Key-Soon Lee who supported with additional presentation. Thank you very much all of you again. I'd like to appreciate so a thank you very much. - 380- JAERI-Conf 99-009

Closing Address

by Key-Soon Lee Director, Nuclear Fuel Examination Team Korea Atomic Energy Research Institute

I would like to express sincere thanks again to Dr. Fujishiro for his help on this Seminar, and Dr. Baba, Mr. Hoshiya and their staffs who have made efforts make this seminar successful. Also we, all of Korean participants, deeply appreciate your kindness and hospitalities rendered to us during our stay at Oarai. I believe that this seminar offered us a good opportunity to exchange information, new ideas, and relevant experiences on PIE technologies, which will benefit the effective promotion of nuclear technology in the next century. And I believe this seminar contributed greatly for us to understand the utilization of PIE facility important again. The 4th KAERI-JAERI Joint Seminar on PIE technology will be held 3years later from now. Then it is going to be the year 2002 of the 21st century. As we know, the year 2002 is the year for the 17th World Cup which Korea and Japan are jointly more meaningful event than ever. Finally, I would like to express my deep appreciation to the JAERI's authority for support of this seminar and have a wonderful dream for the 21st century for all of you. Thank you very much.

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Closing Address by Osamu BABA Vice Chairman of Organizing Committee Director, Department of JMTR, Oarai Research Establishment, JAERI

We have now come to the end of the seminar. Many contributions were made during this seminar for further development in the field of PIE with having totally 66 participants. I hope all of you are satisfied with the seminar, and also enjoyed friendly communications and being stayed in Oarai. Finally, on the behalf of the organizing committee, I wish to express our sincere gratitude to all participants for their contributions to this seminar, and I would like to thank members of the organizing committee for the their assistance to proceed the seminar smoothly. We look forward to seeing many of you again next the 4th KAERI-JAERI joint seminar on PIE technology in KAERI. Now, this brings the 3rd JAERI-KAERI joint seminar on PIE technology to a close.

Thank you.

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Appendix A COMMITTEE

Organizing Committee Chairman : Toshio FUJISHIRO Vice Chairman : Osamu BAB A Member of Committee Yuusuke TOMTTA Tsuneo KODAIRA Norikazu OOKA Taiji HOSHIYA

Program Committee Chairman : Taiji HOSHIYA Member of Committee Hidetoshi AMANO Junichi SATTO Yasuharu NISHINO Hiroyuki KANAZAWA Tadaharu ITO Seiichirou MATSUMOTO Masao OHMI Toshimitsu ISHII

Secretariat Chairman : Taiji HOSHIYA Member of Secretariat Takeshi USUI Keiichirou NISHIWAKI Katsuyuki TOMATSURI Yuuichi NAKAKURA Michio SHIMIZU Tetsuya NAKAGAWA Hideaki MMURA Shigemi IWAMATSU Shizuo SOUZAWA Yoshinobu TAYAMA Hideki TAKADA Kazuo KAWAMATA Yoshiaki KATO Minoru YONEKAWA Taketoshi TAGUCHI Masao OHMI Toshimitsu ISHII Junichi SAITO Izumi SUGIYAMA Mayumi WADA Machiko KOIZUMI

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Number of presentations for the 3rd JAERI-KAERJ seminar on PIE technology

Nation Organization Number of presentation

Korea Atomic Energy Research Institute (KAERI) 12 Korea 13 Hanyang University 1

Japan Atomic Energy Research Institute (JAERI) 10

Japan Nuclear Cycle Development Institute (JNC) 4

Japan Tohoku University 2 20

Nippon Nuclear Fuel Development Co., Ltd. (NFD) 2

Nuclear Development Corporation 2

Total 33

Number of Participants for the 3rd JAERI-KAERI Seminar on PIE Technology

Organization Number of Participant

KAERI 5 6 Hanyang Univ. 1

Tokai 25 71

JAERI Oarai 39 65 Mutsu 1

JNC 5 5

Tohoku Univ. 3 3 13 NFD 3 3

NDC 2 2

Total 84

- 384 - Appendix B Schedule of The 3rd JAERI-KAERI Joint Seminar on PIE

Time 9:00 10:00 11:00 12:00 13:00 14:00 15:00 16:00 17:00 18:00 19:00 20:00 Date I l I r^ i 13:00 14:30 18:30 20:30 Registration *" (9:00-9:30) Reception I I A at A Opening Address 14:40 15:45 (9:40-9:55) lAsahi Bun-shitsu I Of Photo Thursday JNC > 11:30-11:45 m 00 2 00 March 25 en 10:00 11:30 16:00 17:30 n o

O (Presentation) A o (Lunch) I I

Registration (9:00-9:15) II Closing Address 9:15 10:45 13:10 15:00 17:15-17:30 Friday- A A

March 26 17:10 10:55 12:25 15:20 A 1 (Presentation) (Lunch) A JAERI-Conf 99-009

AppendixC l^

The 3rd JAERI-K4ERLlC)iHf SEMINAR on PIE TECHNOLOGY

March 25 * 26, I#9§, Japan AtOfnie Sneff y. Research Institute, Oarai Research Establishment, JAPAN

Thursday March 25

Opening Address 9:40-9:55 Chair person: Norikazu Ooka; JAERI Toshio Fujishiro, Director General, Oarai Research Establishment, JAERI Key-Soon Lee, Director, Nuclear Fuel Cycle Development, KAERI

I. Current status and future perspectives on PIE 10:00-11:30 PIE activity-1 [Chairs: Norikazu Ooka (JAERI) and Key-Soon Lee (KAERI)J 1-1: Over view of nuclear fuel cycle examination facility at KAERI Key-Soon Lee. Eun-Ga Kim, Kih-Soo Joe, Kil-Jeong Kim, Ki-Hong Kim and Duk-Ki Min (KAERI) 1-2: Activities on PIE of nuclear power plant fuels in KAERI Eun-Ka Kim. Yong-Bum Chun, Gil-Sung You, Dae-Seo Koo, Duck-Kee Min Key-Soon Lee and Seung-Gy Ro (KAERI)

1-3: Present status of PIEs in the Department of Hot Laboratories Tsuneo Kodaira. Tomohide Sukegawa, Hidetoshi Amano, Fumio Kanaizuka and Kiyomi Sonpbe (JAERI) 1-4: Current status and future prospects of JMTR Hot Laboratory Osamu Baba. Norikazu Ooka and Taiji Hoshiya (JAERI)

Photo 11:30-11:45 Lunch 11:45-13:20

PIE activity-2 13:20-14:50 [Chairs: Eun-Ka Kim (KAERI) and Tsuneo Kodaira (JAERI)] 1-5: Over view of post?irradiation examination facilities for fuels and materials development of fast reactor Masahiko Itoh (JNC)

OOO JAERI-Conf 99-009

The 3rd JAERI-KAERI JOINT SEMINAR on PIE TECHNOLOGY

March 25 - 26, 1999, Japan Atomic Energy Research Institute, Oarai Research Establishment, JAPAN

I-6(a): Activities of Oarai Branch IMR ofTbhoku University as an open facility for utilizing JMTR Minoru Narui. Tsutomu Sagawa and Tatsuo Shikama (Tohoku Univ.) I-6(b): Ventilation system of actinides handling facility in Oarai-Branch of Tohoku University Yoshimitsu Suzuki. Makoto Watanabe, Mituo Hara, Tatsuo Shikama Hideo Kayano and Toshiaki Mitsugashira (Tohoku Univ.) 1-7: PIE activities in NFD Hot Laboratory Norikatsu Yokota, Keizo Ogata and Noriyuki Sakaguchi (NFD) 1-8: Current status of NDC Fuel Hot Laboratory Youichirou Yamaguchi. Takanori Matsuoka, Satoshi Shiraishi and Mitsuteru Sugano (NDC)

II. PIE techniques Elementary techniques for the study of power reactor 15:00-16:05 [Chair: Norikazu Ooka (JAER1)] II-1: Development and application of PIE apparatuses for high-bumup LWR fuels Katsuya Harada. Naoaki Mita, Yasuharu Nishino and Hidetoshi Amano (JAERI) II-2: A technique of melting temperature measurement and its application for irradiated high-burnup MOX fuels Takashi Namekawa and Takashi Hirosawa (JNC) II-3: Development of PIE techniques for irradiated LWR pressure vessel steels Masahiro Nishi, Minoru Kizaki and Tomohide Sukegawa (JAERI)

Microstructural and Quantitative analysis 16:20-17:50 [Chairs: Takanori Matsuoka (NDC) and Sang-Bok Ahn (KAERI)] II-4: High resolution grain boundary analysis of neutron irradiated stainless steel using FEG-TEM Mitsuhiro Kodama. Yoshihide Ishiyama and Norikatsu Yokota (NFD) II-5: The development of crack measurement system using the direct current potential drop method for use in the hot cell Do-Sik Kim, Sang-Bok Ahn. Key-Soon Lee, Yong-Suk Kim and Sang-Chul Kwon ( KAERI)

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SEMINAR on PIE TECHNOLOGY

March 25 - 26,1999, Japan Atomic Eriergy Research Institute, Oarai Research Establishment, JAPAN

II-6: Development of k remote controlled small punch testing machine for nuclear fusion research Masao Ohml. Junichi Saito, Toshimitsu Ishii, Taiji Hoshiya and Shiro Jitsukawa (JAERI) II-7: Newly developed non-destructive testing method for evaluation of irradiation brittleness of structural materials using ultrasonic Toshimitsu Ishii. Norikazu Ooka, Yoshiaki Kato, Junichi Saito, Taiji Hoshiya (JAERI) Saburo Shibata (IHI) and Hideo Kobayashi (Tokyo Institute of Technology)

Reception 18:30-20:30

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The 3rd JAERI-KAERI JOINT SEMINAR on PIE TECHNOLOGY

March 25-26,1999, Japan Atomic Energy Research InMitutc. Oarai Research Establishment, JAPAN

Friday March 26

Assembling and utilization techniques 9:15-10:45 [Chairs: Keizo Ogata (NFD) and Yong-Sun Choo (KAERI)] 11-8; Reassembling technique for irradiation vehicle at Fuel Monitoring Facility (FMF) Koji Maeda. Tsuyoshi Nagamine, Yasuo Nakamura, Takeshi Mitsugi and Shinichiro Matsumoto (JNC) n-9: The development of electric discharge machine for hot cell usage Wan-Ho Oh, Sang-Bok Ahn. Sang-Chul Kwon, Yong-Suk Kim and Key-Soon Lee (KAERI) II-10: Development of remote laser welding technology , . Soo-Sung Kim, Woong-Ki Kim, Jung-Won Lee, Myung-Seung Yang and Hyun-Soo Park (Yong-Sun Chool (KAERI) II-11: SEM modification and shielded glove box design for the radioactive material Ki-Seog Seo, Jeong-Hoe Ku, Kyoyng-Sik Bang, Ju-Chan Lee, Gil-Sung You Dac-Seo Ku and Duck-Kee Min (Dac-Seo Koo*> (KAERI)

III. Evaluation of PIE data Irradiation effects of in-core component 10:55-12:25 (Chairs: Eun-Ka Kirn; KAERI and Takashi Tsukada; JAERI) III-1: Detection of defects in control rods by eddy current examination Dae-Seo Koo. Jeong-Hoe Ku, Duck-Kee Min, Ro Seung-Gy, Young-Sang Joo and Yoon-Kyu Park (KAOT) III-2: Life time estimation for irradiation assisted mechanical cracking of PWR RCCA rodlets Takanori Matsuoka and Youichirou Yamaguchi (NDC) III-3: Surveillance tests for Jtight-water cooled nuclear power reactor vessels in IMEF Yong-Sun Choo. Sang-Bok Ahn, Dae-Gyu Park, Yang-Hong Jung Byung-Ok Yoo, Wan-Ho Oh, Seung-Je Baik, Dae-Seo Koo and Key-Soon Lee (KAERI) III-4: The fracture toughness testing of unirradiated and irradiated Zr-2.5Nb CANDU pressure tube Sang-Bok Ahn. Do-Sik Kim, Dae-Seo Koo, Sang-Chul Kwon and Yong-Suk Kim (KAERI)

Lunch 12:25-13:10

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March 25 - 26, 1999, Japan Atomic Energy Research Institute, Oarai Research Establishment, JAPAN

Fundamental behavior of driver fuels 13:10-15:00 [Chairs: Keizo Ogata (NFD) and Takanori Maruyama (JNC)] HI-5: Post-irradiation examination of PWR fuels in KOREA Young-Bum Chun, Gil-Sung You, Dae-Seo Koo, Eun-Ka Kim. Duck-Kee Min and Seung-Gy Ro (KAERI) HI-6: Hydriding failure analysis based on PIE data Yong-Soo Kim (Hanyang Univ.), Hyun-Taek Park, Hwee-Soo Jun (Korea Electric Power Corp.) Yong-Bum Chun, Gil-Sang You, Duck-Kee Min Eun-Ka Kim and Seung-Gy Ro (KAERI) III-7: Re-irradiation tests of spent fuel at JMTR by means of re-instrumentation technique Jinichi Nakamura. Michio Shimizu, Yasuichi Endo, Hideaki Nabeya Kenichi khise, Junichi Saito, Kunio Oshima and Hiroshi Uetsuka (JAERI) III-8: HANARO fuel gamma scanning Kwon-Pyo Hong, Tae-Yon Kim, Dae-Gyu Park, Dae-Seo Koo and Bong-Goo Kim fKey-Soon Lee) (KAERI) III-9: Metallurgical properties of power reactor fuels after irradiation Gil-Sung You, Hang-Suk Seo, Sung-Ho Eom, Duek-Kee Min, Eun-Ka Kim Dae-Seo Koo and Jun-Sik Ju (KAERI)

R&D for the next decade and users' requirements for PIE 15:20-17:10 [Chairs: Tatsuo Shikama (Tohoku Univ.) and Yong-Soo Kim (Hanyang Univ.)] Ill-10: Post irradiation examinations for IASCC study at JAERI Takashi Tsukada. Yukio Miwa, Hirokazu Tsuji and Hajime Nakajima (JAERI) III-ll: Determination of irradiation temperature using SiC temperature monitors Tadashi Maruyama and Shoji Onose (JNC) III-12: R&D status and requirements for PIE in the fields of the HTGR fuel and the innovative basic research on high-temperature engineering Kazuhiro Sawa. Masahiro Ishihara, Tsutomu Tobita, Junya Sumita Kimio Hayashi. Taijf Hoshiya, Hajime Sekino and Etsurou Ooeda (JAERI)

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The 3rd JAERI-KAERI JOINT SEMINAR on PIE TECHNOLOGY

March 25 - 26, 1999, Japan Atomic Energy Research Institute, Oarai Research Establishment, JAPAN

HI-13: Advanced post irradiation examination for fusion reactor development in JMTR Kunihiko Tsuchiya. Etsuo Ishitsuka, Minoru Uda, Junichi Saito and Hiroshi Kawamura (JAERI) III-14: Hot cell works and related irradiation tests in fission reactor for development of new materials for nuclear application Tatsuo Shikama (Tohoku Univ.)

Closing 17:15-17:30 [Chair: Norikazu Ooka (JAERI)] Key-Soon Lee, Director, Nuclear Fuel Cycle Development, KAERI Osamu Baba, Director, Department of JMTR, JAERI

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The 3rd JAERI - KAERI Jpjrit Seminar on PIE Technology

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In the seminar room (Meeting room of H'l'l'R)

Welcome to Hie 3rd JAERI •• KAER! Joint Seminar on Pit Technology

In the reception room (Asahi bun-shitsu of JNC Oarai)

The 3rd JAERI - KAERI Joint Seminar on PIE Technology March 25-26,1999, JAERI Oarai, Japan

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