Nuclear Science User Facilities FY 2017 Annual Report

Nuclear Science User Facilities

Unloading an experiment at the Hot Fuel Examination Facility (HFEF), Materials and Fuels Complex (MFC), INL (Chris Morgan, INL)

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Nuclear Science User Facilities 995 University Boulevard Idaho Falls, ID 83401-3553 nsuf.inl.gov

Disclaimer This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the U.S. Government nor any agency thereof, nor any of their employees, makes any warranty, expressed or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. References herein to any specific commercial product, process, or service by trade name, trade mark, manufacturer, or otherwise, does not necessarily constitute or imply its endorsement, recommendation, or favoring by the U.S. Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the U.S. Government or any agency thereof. INL/EXT-_ _-_ _ _ _ Prepared for the U.S. Department of Energy, Office of Nuclear Energy under DOE Idaho Operations Office Contract DE-AC07-051D14517.

(This report covers the period beginning October 1, 2016, through September 30, 2017)

Cover Image: A model of the Advanced Test Reactor (ATR) produced by advanced simulation capabilities at Idaho National Laboratory (INL). Nuclear Science User Facilities

OUR NSUF TEAM

Dan Ogden Brenden Heidrich Jeff Benson Deputy Director Chief Irradiation Scientist Program Administrator (208) 526-4400 (208) 533-8210 (208) 526-3841 [email protected] [email protected] [email protected]

Simon Pimblott Collin Knight Lindy Bean Chief Post-irradiation Post-irradiation Planning and Financial Scientist Examination Project Manager Controls Specialist (208) 526-7499 (208) 533-7707 (208) 526-4662 [email protected] [email protected] [email protected]

Keith Jewell Katie Anderson Travis Howell J. Rory Kennedy Technical Lead Experiment Manager Planning and Financial Director (208) 526-3944 (208) 526-0049 Controls Specialist (208) 526-5522 [email protected] [email protected] (208) 526-3817 [email protected] [email protected]

Nicholas Meacham Thomas Maddock Renae Soelberg Experiment Manager Technical Lead Administrative Assistant (208) 526-3227 (International) (208) 526-6918 [email protected] (208) 526-2714 [email protected] [email protected]

Jonathan Kirkham John Coody Nuclear Energy Infrastructure Project Scheduler Database Coordinator (208) 526-2964 (208) 533-8188 [email protected] [email protected]

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Brenden Heidrich Jeff Benson John Jackson Chief Irradiation Scientist Program Administrator Industry Program Lead (208) 533-8210 (208) 526-3841 (208) 526-0293 [email protected] [email protected] [email protected]

Collin Knight Lindy Bean Kelly Cunningham Post-irradiation Planning and Financial Nuclear Fuels and Materials Examination Project Manager Controls Specialist Library Coordinator (208) 533-7707 (208) 526-4662 (208) 526-2369 [email protected] [email protected] [email protected]

Katie Anderson Travis Howell Laura Scheele Experiment Manager Planning and Financial Communications Liaison (208) 526-0049 Controls Specialist (208) 526-0442 [email protected] (208) 526-3817 [email protected] [email protected]

Thomas Maddock Renae Soelberg Technical Lead Administrative Assistant (International) (208) 526-6918 (208) 526-2714 [email protected] [email protected]

John Coody Project Scheduler (208) 526-2964 [email protected]

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Radiological Technician operating remote manipulator arms, Westinghouse Churchill Site High-level Hot Cell (Courtesy of Westinghouse Electric Company)6 2017 | ANNUAL REPORT

TABLE OF CONTENTS

Nuclear Science User Facilities • From the NSUF Director...... 9 • NSUF Timeline...... 16 • DOE-ID Program Manager Retires...... 21 • Focus on New Staff...... 22 • NSUF Summer Interns...... 33

NSUF Overview • NSUF Researcher Profiles...... 36 • Peter Hosemann ...... 36 • Riley Parrish ...... 40 • Luca Capriotti ...... 44 • Fidelma Di Lemma ...... 46 • The Glovebox...... 50 • New NSUF Partners...... 53 • NSUF-GAIN Synergy...... 60 • Measuring Impact...... 62 • Table of FY 2017 Awarded Projects...... 68

NSUF Across the Nation • Map of NSUF Partner and User Institutions...... 86 • NSUF User Institutions...... 87

NSUF Awarded Projects • Project Reports...... 89

Resources • Acronyms...... 157 • Index...... 162 Nuclear Science User Facilities

Laser Welder at the Test Train Assembly Facility, Advanced Test Reactor (ATR) Complex, Idaho National Laboratory (INL) (Steve Gamache, INL) 8 2017 | ANNUAL REPORT

FROM THE NSUF DIRECTOR

J. Rory Kennedy Director (208) 526-5522 [email protected]

he Nuclear Science User proposals were received from 48 Reactor-2 (BR-2) and associated Labo- Facilities (NSUF) celebrated our institutions in FY 2017 (a 140 percent ratory for High and Medium Activity 10th anniversary in 2017, a year increase from FY 2016), from which (LHMA). Department of Energy T th that also marked the 50 anniversary 92 projects were awarded (a 136 (DOE) and SCK•CEN signed a Memo- of the Advanced Test Reactor (ATR), percent increase from FY 2016). randum of Understanding (MOU) the founding facility of the NSUF. concerning cooperation in nuclear Seven new partner facilities were energy research and development in Fiscal year (FY) 2017 was another accepted into the NSUF. The parent January 2017. This MOU established exceptional year for the NSUF in a institutions include Brookhaven the basis for in-kind collaboration on number of areas. The demand for National Laboratory, Lawrence projects of mutual interest, employing NSUF award opportunities continued Livermore National Laboratory, Los the BR-2 and LHMA together with to expand. The Consolidated Innova- Alamos National Laboratory, Sandia the ATR, the Transient Reactor Test tive Nuclear Research (CINR) Funding National Laboratories, The Ohio State (TREAT) Facility, and associated facili- Opportunity Announcement (FOA) University, University of Florida, and ties located at Idaho National Labora- solicitation results saw, once again, Texas A&M University. The NSUF has tory (INL), as well as other facilities the NSUF achieving record numbers: now evolved to include 20 partner that are part of the NSUF. 124 Letters of Intent (LOIs) leading facilities with each facility bringing to 108 preproposal submissions from exceptional capabilities to the relation- The steady growth in the number which 50 full proposals were invited. ship, including: reactors, beamlines, of NSUF partners led to the NSUF $11 million in direct project funding instruments, hot cells, and impor- hosting the first NSUF Partner allowed us to award 15 projects tantly, technical and scientific expertise Facilities Working Group meeting, ranging in cost from $60,000 to with the capabilities that are so critical May 24-25, 2017, at the Center for $3.6 million. Five of the 15 awards to obtain quality results. Advanced Energy Studies (CAES) in went to industry leads, five went to Idaho Falls, Idaho. The working group The NSUF also added our first university leads, and five went to meeting was intended to provide the international affiliate, Belgium’s national laboratory leads. The NSUF partner facilities with an avenue to Studiecentrum voor Kernenergie/ also saw a record number of self-organize in order to increase their Centre d’Etude de l’Energie Nucléaire applications and awards for the involvement in programmatic activities (SCK•CEN) Belgian Nuclear Research FY 2017 Rapid Turnaround Experi- and to establish a baseline for evalu- Centre that houses the Belgium ments (RTEs). A total of 180 RTEs ating shared interests and concerns

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among the participating institutions. Laura Scheele joined the NSUF as workshop objective was to develop The meeting was well-attended and communications liaison, replacing a ranked list of thermal-hydraulic quite educational with respect to the Sarah Robertson, who moved to research and development needs in the partner facilities gaining a better under- another position. We will miss Sarah reactor technology areas of light water standing of the breadth of capabilities but know our communications are in reactors, fast reactors, high-temperature and activities of the NSUF. good hands with Laura. She previously gas reactors, and molten salt reactors. handled media relations for INL and The workshop was well-attended with We welcomed three new NSUF has worked for the American Nuclear approximately 70 participants from team members in FY 2017. After Society in a communications and national laboratories, universities, two years of searching, our chief public policy role. Please feel free to industry and foreign nuclear organiza- post-irradiation scientist position contact her with any questions about tions, as well as Department of Energy was finally filled by Simon Pimblott, the NSUF and plan to see her at several Office of Nuclear Energy (DOE-NE) Ph.D. Simon comes to us from the of our conference exhibits. and Department of Energy Idaho Oper- United Kingdom, where he was ations Office (DOE-ID). The NSUF’s Chaired Professor of Radiation The NSUF has also increased dedicated industry programs will continue to Chemistry at Manchester University technical resources to support the evolve as we ensure that proposals and founding director of the Dalton ever-growing demand for projects. focus on priority areas to support Cumbrian Facility. Simon was already Keith Jewell, Ph.D., has transitioned today’s reactor fleet and tomorrow’s quite familiar with the NSUF, having into a full-time technical lead, and energy systems. The NSUF will remain served as the international member the NSUF has secured the expertise a key contributor to and supporter of of the NSUF Science Review Board of Nick Meacham and Katie Anderson the GAIN initiative in its charge to aid since 2012. One of his tasks in FY as full time experiment managers. industry in accelerating innovation. 2018 will be to measure the overall Tom Maddock will remain a part-time Through our solicitation processes, the research impact of the NSUF over the technical lead (international). The NSUF offers the opportunity to address last 10 years. NSUF continues to seek technical leads and solve targeted issues of importance to partner with principal investigators With the steady addition of new to the nuclear industry. (PIs) to plan and execute experi- partner facilities and demand for ments to ensure that research projects In a first-of-its-kind endeavor, the NSUF funding opportunities, we proceed smoothly and according NSUF brought together experts and foresaw the need for an additional to schedule. It is important to note stakeholders in the area of ion beam planning and financial control that the NSUF technical leads are irradiations to prepare a document specialist. Travis Howell now fulfills scientific professionals, and I thank addressing the application of ion this essential role for the NSUF. His our supported PIs for recognizing this beam technologies to advancing work experience includes three years by having the technical leads become nuclear energy. The work is titled, at an engineering, fabrication, and scientifically and technically involved “Roadmap for the Application of Ion manufacturing company managing in the projects NSUF supports. Beam Technologies to Challenges for projects constructing components the Advancement and Implementa- for the commercial nuclear sector. The NSUF furthered our efforts in our tion of Nuclear Energy Technologies,” He assists NSUF managers in making charge from DOE-NE to provide infor- and should be available to the public strategic operational decisions in an mation to best manage infrastructure in early FY 2018. Again, this is the efficient and productive manner. when we teamed with the Gateway first such road map addressing the for Accelerated Innovation in Nuclear issue that we are aware of and we (GAIN) and co-hosted a thermal expect it to have a significant impact hydraulics workshop in July 2017. The on the field.

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Gamma Irradiation Test Loop, Fuels and Applied Science Building (FASB), MFC, 12 INL (Chris Morgan, INL) 2017 | ANNUAL REPORT

Building upon the continued success project knowledge, including refer- research. Now reaping the benefits of and growth of the Nuclear Fuels and ences and links, where appropriate, to 10 years of NSUF-supported research, Materials Library (NFML) and the publications and reports that contain the American Nuclear Society (ANS) Nuclear Energy Infrastructure Data- the information and knowledge Materials Science and Technology base (NEID) – and the goal to provide gained from those projects. Division organized, together with a completely integrated web-based the NSUF, three NSUF sessions at the The NSUF maintained an active suite of research tools – the NSUF 2017 ANS Annual Meeting, during presence at scientific conferences and established the Combined Materials which 18 NSUF-supported research meetings. By expanding awareness Experiment Toolkit (CoMET). It will papers were presented. The NSUF of the opportunities and capabilities eventually not only link the NFML and exhibited and was invited to present provided by DOE-NE through the NEID, but also databases of scientific at several conferences and meetings in NSUF, we increased the impact and technological expertise and the U.S. (See Table 1) and recognition of NSUF-awarded

Table 1.

NSUF Conference and Meetings Engagement: FY 2017 NSUF Exhibits Nuclear Materials Conference (NuMat) American Nuclear Society (ANS) Winter Meeting Materials Research Society Winter Meeting ANS Student Conference The Minerals, Metals and Materials Society (TMS) Annual Meeting Environmental Degradation Conference NSUF Invited Presentations Advanced Sensors and Instrumentation Program review GE Hitachi Advanced Manufacturing Works EPRI Primary Systems Corrosion Technical Advisory Committee Accelerator Applications in Research and Industry Conference Toshiba/CRIEPI “U-Free” TRU Burner Concepts meeting China National Nuclear Corporation (CNNC) Nuclear Power Institute of China (NPIC) meeting U.S. Nuclear Regulatory Commission (NRC) Materials Harvesting Workshop Montana State University 4th Technical Meeting of the Advanced Reactor Research and Development, Fuel Cycle Research and Development and Waste Management, and Light-Water Reactor Research and Development Sub-Working Groups of the Civil Nuclear Energy Research and Development Working Group (CNWG) INL/ORNL ICERR Assessment MeV Summer School DOE-NE Cross-cut Coordination meeting National Organization of Test, Research, and Training Reactors (TRTR) Conference Utilities Service Alliance

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International interest in the structure time on INL’s Falcon, an SGI ICE-X and work of the NSUF is growing. distributed memory system with Our unique distributed partnership 34,992 cores, 121 terabytes of model, as well as our NFML and memory and a LINPACK rating of NEID, are increasingly being consid- 1,087 teraflops. HPC supports a wide ered by other countries. The NSUF range of research activities, including was invited to present at the Nuclear performance of materials in harsh Materials Conference in France, the environments (including the effects Hot Lab Conference in Japan, the of irradiation and high temperatures) Global Conference in South Korea, and multiscale multiphysics analysis “As we move into and the Nuclear Academics Discus- of nuclear fuel performance. I sion Meeting (NADM) in England. In strongly encourage our users and the FY 2018, the NSUF will addition to representing the NSUF, nuclear community to take advantage these events provide the opportunity of this capability. to assess international capabilities Please take a few moments to read continue to build upon its and resources that may be of interest through this report and familiarize to the NSUF community. yourself with our organization, foundational success.” As we move into FY 2018, the our research, and the opportunities NSUF will continue to build upon available through the NSUF. We put its foundational success. We must a good amount of effort into our continue to invest in the capabilities, annual reports to keep our users resources, and scientific expertise informed, and take great pride in needed to support the anticipated them. As a note of recognition, the growth in CINR and RTE projects. NSUF 2015 Annual Report received We will continue to enhance and an Award of Distinction in the 2017 streamline the NEID and NFML Communicator Competition, as and to expand them into CoMET judged by the Academy of Interac- to provide seamless information tive and Visual Arts. I thank the management for researchers. NSUF staff, partners, users, and both DOE-NE and DOE-ID for their hard High Performance Computing work to make the NSUF a successful (HPC) is a valuable offering available strategic research asset. through the CINR and RTE calls. The NSUF is making available approximately 30 percent of computing

J. Rory Kennedy

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Bryan Forsmann, Center for Advanced Energy Studies (CAES), preparing samples in the Materials Laboratory, CAES (Chris Morgan,15 INL) Nuclear Science User Facilities

NSUF TIMELINE

2007 2008 2009

The NSUF (INL) MIT joins CAES joins North Carolina established as the NSUF – the NSUF – State University DOE-NE’s first Neutron Low Activity joins the NSUF user facility – Irradiation Laboratories – Beamline Neutron (positron), Irradiation, Neutron Hot Cells, Irradiation Gamma Irradiation, Low Activity Laboratories

Illinois Institute University of of Technology Michigan joins the joins the NSUF – NSUF – Beamline Beamline (x-ray) (ion), Hot Cells

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University of Nevada, Las Vegas Purdue University joins the NSUF joins the NSUF – – Low Activity Beamline (ion) Laboratories

Oak Ridge National Pacific Northwest Laboratory joins the National University of NSUF – Neutron University of Laboratory Wisconsin joins the Irradiation, Gamma California, Berkeley joins the NSUF NSUF – Beamline Irradiation, Hot joins the NSUF – Hot Cells, (ion), Low Activity Cells, Low Activity – Low Activity Low Activity Laboratories Laboratories Laboratories Laboratories

2010 2011 2012

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Sandia National Laboratories joins the NSUF – Gamma Irradiation, Neutron Irradiation, Beamline (ion)

Westinghouse Argonne Brookhaven joins the NSUF INL offers High National National – Hot Cells, Low Performance Laboratory joins Laboratory joins Activity Computing the NSUF – the NSUF – Laboratories capabilities Beamline (ion) Beamline (x-ray)

2013 2015 2016 2017

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Los Alamos The Ohio State SCK•CEN joins National University the NSUF as the Laboratory joins the NSUF first international joins the NSUF – Neutron affiliate – – Beamline Irradiation Neutron (neutron), Irradiation, Hot Cells, Hot Cells, Low Activity Low Activity Laboratories Laboratories

Lawrence University of Texas A&M joins Livermore Florida joins the NSUF – National the NSUF – Beamline (ion) Laboratory joins Low Activity the NSUF – Laboratories Beamline (ion)

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Researcher Ziqing Zhai, Quanta Focused Ion Beam (FIB) microscope, Materials Science and Technology Laboratory (MSTL), Pacific Northwest National Laboratory (PNNL) (Courtesy of PNNL) 20 2017 | ANNUAL REPORT

DOE-ID PROGRAM MANAGER RETIRES

Brooks Weingartner reflects on his time overseeing the NSUF

“Verify and validate” were the key “Rory has assembled a first-rate team words for Brooks Weingartner in the and they are doing first-rate work,” time he was the U.S. Department of he said. The most gratifying aspect Energy’s Idaho Operations Office of the job was “seeing the breadth point man for contractual oversight of work across the nation and how it of programs including the Nuclear supported DOE-NE’s mission.” Science User Facilities (NSUF). “Rory has assembled a Established at Idaho National Labora- Weingartner retired from his position tory in 2007, the NSUF expanded at the end of 2017, looking forward to partner facilities outside INL the first-rate team and they are to returning to environmental engi- following year and has continued to do neering, his original field of expertise. so into 2018. If there is one particular He received a bachelor’s in geological challenge for the NSUF, it is balancing doing first-rate work.” engineering from Montana Tech of the the resources with the increasing University of Montana in 1988 and a interest in and demand for new master’s in environmental engineering funding awards to facilitate research. there in 1992. “As the NSUF has acquired new He took his DOE job as NSUF partner facilities to expand the capa- program manager in 2013, about bilities available to researchers, the pie the same time as NSUF Director has stayed the same size,” said Wein- Rory Kennedy came in to oversee the gartner. “Even though the funding has NSUF. Weingartner’s responsibilities stayed flat, the number of proposals included helping to put together has been growing. That’s good news work packages and keeping track in terms of the high demand for of milestones. The time he spent as NSUF capabilities, but it also requires DOE-Idaho’s program manager gave a strategic approach to addressing him some special insight. research gaps.”

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FOCUS ON NEW STAFF Simon Pimblott NSUF Chief Post-Irradiation Scientist nterested in the future of research Pimblott was well-suited to provide priorities? Spend a few minutes an international perspective. He hails Iwith Simon Pimblott, the NSUF from Derby, Great Britain. His interest Chief Post-Irradiation Scientist and in nuclear energy was sparked when INL Directorate Fellow, who joined the he received a scholarship to St. Peter’s NSUF in September 2017. His involve- College at the University of Oxford ment with the NSUF began about five from the U.K. Central Electricity years earlier, in 2012, when then- Generation Board. NSUF Director Todd Allen recruited “The scholarship required me to him as the international member of work on CEGB projects prior to going the NSUF Science Review Board. to university and during the summer The NSUF Science Review Board vacations,” explains Pimblott. “My provides independent overview and first project was to study SOX and input to the NSUF on the broad range NOX production by fossil fuels and of NSUF programs and initiatives their contributions to acid rain. My to provide access to nuclear energy introduction to nuclear was on a research capabilities, to generate project at Berkeley Nuclear Laborato- impactful results and to maintain ries, on the use of low oxidation state and enhance the infrastructure, metal ions for the decontamination capabilities and expertise available in of steam generator pipework. This the United States. An international work provided me with technical perspective on the Science Review insight into the benefits of generation Board is essential to maintaining the that doesn’t rely upon combustion, NSUF’s status as DOE-NE’s world- with fission generation being the class user facilities organization. most robust.” “The United States has to understand Pimblott pursued his doctorate how the international community (D.Phil.) in the Physical Chemistry prioritizes, maintains and uses nuclear Laboratory at the University of energy research capabilities,” said Oxford and at Harwell with a scholar- Pimblott. “Getting international ship from the U.K. Atomic Energy feedback helps DOE-NE and the NSUF Authority. Following his D.Phil., drive strategic decisions on research infrastructure priorities.”

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Ph.D. students Bill Chuirazzi (left) and Ibrahim Oksuz (right), Nuclear Reactor Laboratory, The Ohio State University Research Reactor (OSURR), The Ohio State University (Courtesy of The Ohio State University) 23 Nuclear Science User Facilities

Researchers, XPD Beamline, National Synchrotron Light Source (NSLS) II, Brookhaven National Laboratory (BNL) 24 (Courtesy of BNL) 2017 | ANNUAL REPORT

Pimblott joined the Radiation Labora- psychology research that indicated tory and later the Department of that role preparation plays a bigger Physics at the University of Notre part than innate talent in the careers of Dame. Among his motivations for the gifted. In cognitively demanding making the move? “I wanted to see fields, 10,000 hours (or 10 years), the United States,” he said. seems to be a rule of thumb for the amount of time necessary to excel at He not only saw the United States, complex tasks. but he met Nancy “Hedge” Harridge, “The NSUF today provides his future wife, while attending a Pimblott takes this notion to heart. radiation research conference in “I spent eleven years building Dalton world-leading science Nashville, Tennessee. Pimblott says Cumbria into a multidisciplinary and he and Hedge have been married too financially solvent laboratory,” said many years to count. Their family Pimblott. “The timing was right for and engineering research has grown to include two daughters me to move into a new position with Robyn and Erin, plus two sons-in-law new opportunities and challenges and five grandchildren who live in that match my expertise.” The NSUF capabilities. The key is to Ohio and Tennessee. offered a perfect fit. Always ready for challenge, Pimblott He has seen the NSUF experience strategically balance NSUF left Notre Dame in 2006 to establish dramatic growth over the past the Dalton Cumbrian Facility for 10 years. “The NSUF offers a broader capabilities to fulfill emerging The University of Manchester and range of capabilities. Now the NSUF the U.K. Nuclear Decommissioning is way beyond reactor experiments Authority. The laboratory initially and is active in simulation, analysis research needs.” focused on radiation effects on and the interrogation of irradiated materials and robotics for use in materials,” said Pimblott. “The NSUF nuclear facilities and grew under today provides world-leading science Pimblott’s leadership to include work and engineering research capabilities. in fuel cycle, water chemistry, waste The key is to strategically balance packaging, nuclear fuel performance NSUF capabilities to fulfill emerging and reprocessing chemistry. research needs.” Malcom Gladwell, in his book “Outliers,” popularized the notion that achievement is talent plus preparation. The concept is based on

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Travis Howell Minding the Numbers

ehind every experiment is Howell’s focus is on the numbers, someone whose job it is to not the engineering. In the planning Bkeep track of the money. and setting up of any experiment, Even before the addition of six new milestones are scheduled. As partner facilities in 2017, directors milestones are met, Howell’s job is of the Nuclear Science User Facilities to communicate with experiment (NSUF) knew they were going to managers to provide planning need an extra planning and financial and controls support to assigned control specialist (PFC). projects. Howell provides a wealth of services, including supporting Travis Howell, a native of Blackfoot, the development, implementation, Idaho, was brought into the NSUF analysis, and monitoring of scope, fold at the beginning of 2017 to help schedule, budget and cost; and handle the planning and finances ensuring cost plus commitments for a rising number of experiments. do not exceed approved funding Howell earned his MBA with an ceilings. PFCs also assist with emphasis in finance from Idaho proposal preparation and State University in 2013. His work development of cost estimates; experience includes three years at preparing monthly performance an engineering, fabrication and reports and confirming that the manufacturing company, where actual cost is appropriate and he managed projects involving the correct for designated work construction of components for the scope; and implementing project commercial nuclear sector. Howell closeout procedures. then spent one year doing cost analysis and accounting for a health and wellness company. Both of these positions cultivated proficiencies required in his current role at INL within the NSUF.

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Keyou Mao, Purdue University, using the Transmission Electron Microscope, Microscopy and Characterization Suite, CAES27 Nuclear Science User Facilities

Loading a non-fueled test, Laser Welder, TTAF, ATR Complex, INL 28 (Steve Gamache, INL) 2017 | ANNUAL REPORT

Communication with work scope results driven. They really want to managers and other business make a difference in our world’s management staff is essential to energy future. Working with people “The NSUF has a great team success. There must be a foundation like that is contagious. The NSUF is of trust and respect which enables a great program and I feel extremely of individuals that are very work scope managers and PFCs to fortunate to be a part of it.” work in tandem using individual Growing up in eastern Idaho, aptitude and training to aid project Howell says he’d always been aware passionate about what they achievement. His work also requires of Idaho National Laboratory and knowledge and use of a wide array the fact that nuclear research was do. They are customer focused of business systems. These applica- conducted there. But seeing the tions assemble a large amount of projects and meeting the people has information and help PFCs organize given him a deeper understanding. and results driven. They really it into a manner that can assist “I didn’t grasp the magnitude and managers in making strategic, importance of INL’s research and want to make a difference in prudent and operational decisions in mission until I had the opportunity an efficient and productive manner. to witness the focus and drive of Working at the NSUF has been a world class scientists, researchers, our world’s energy future.” revelation for Howell. “I enjoy the managers and support staff with a people,” he said. “The NSUF has a common goal,” he explained. great team of individuals that are very passionate about what they do. They are customer focused and

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Laura Scheele Getting the Word Out

hile she has had an appre- public and environmental policy at ciation for nuclear energy the University of Colorado. She was Wsince she was getting her attracted to nuclear energy because of master’s, it’s only been the past year “the elegance of the fission process” that Laura Scheele has taken a deep dive and the benefits of a baseload energy into to the workings of how the wheels source that didn’t put massive amounts turn at the most basic level. of carbon dioxide into the atmosphere. Scheele became communications lead From 2008 to 2012 she was commu- for Nuclear Science User Facilities nications and policy manager for the (NSUF) in January 2017. The previous American Nuclear Society, managing two years she had been media relations media relations and developing lead for Idaho National Laboratory. strategic messaging, especially in In that job, the focus was wider, on the rapidly emerging world of social getting word out to the world about media. She moved to Richland, Wash- the work going on at the lab. At the ington, in 2013 to become senior NSUF, she has learned a lot more about public affairs analyst and external how nuclear energy research happens relationship manager for Energy and how the U.S. Department of Energy Northwest, a 27-member public supports it. power consortium. “I went from a high level appre- In the course of her career, Scheele said ciation of it to a more nuts-and-bolts she has seen a shift in the prospects for understanding of what goes on in the nuclear energy. “I think it has changed industry,” she said. a lot as millennials come into their own. Younger people, they see climate She has become more adept at web change and the threat it poses, and layout. “You have to get the news up they’re more open to technological fast,” she said. “It can get very busy solutions like nuclear energy. You when you’ve got three calls for rapid see a lot of interest and excitement turnaround experiments each year, as about new innovations, and the NSUF well as major research and infrastruc- supports a lot of the research that will ture projects.” get us there.” A native of Indiana, part of the greater Chicago area, Scheele earned her bachelor’s in political science from Vassar College. She then studied

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Removing a fuel element during a routine refueling operation, High Flux Isotope Reactor (HFIR), Oak Ridge National Laboratory (ORNL) (Courtesty of ORNL) 31 Nuclear Science User Facilities

Megan Isabelle, KaeCee Holden, and Kelly Verner, NSUF Interns, 32 CAES (Chris Morgan, INL) 2017 | ANNUAL REPORT

NSUF SUMMER INTERNS

NSUF interns power summer research work When they began their 2017 Nuclear and the world,” said Holden, who Science User Facilities (NSUF) grew up in central Kansas. She became summer internships, KaeCee Holden, fascinated with all things nuclear Megan Isabelle and Kelley Verner were during her sophomore year chemistry somewhat surprised to find them- class in high school. She earned her selves without male colleagues in their bachelor’s in applied physics, with select group. an emphasis in nuclear science and a minor in astronomy, from Brigham At school – the University of Idaho Young University in 2016, and is (UI) for Holden and Verner, North I believe nuclear power now working on a master’s in nuclear Carolina (NC) State for Isabelle – engineering at University of Idaho – they’d been in the minority. While not Idaho Falls. will be an essential component dwelling on this – they had work to do, after all – they inadvertently hit Isabelle got interested in nuclear on an issue the nuclear industry has research in high school when she was in the future energy noticed and is seeking to address. in NASA’s Virginia Aerospace Science and Technology Scholars program. “One of the most important things production of the United They planned, designed and evaluated we can do is to encourage outstanding a manned mission to Mars. “With any women scientists and engineers to manned deep space mission, radiation States and the world.” enter and to remain in our field,” said is of the highest concern, which is Richard Lester, head of Massachu- how I found myself studying nuclear setts Institute of Technology (MIT’s) engineering,” she said. Her fascination — Kaecee Holden, University of Nuclear Science & Engineering grew at NC State University, where she Idaho and NSUF Summer Intern Department, at a 2015 symposium. became interested in someday partici- The enthusiasm Holden, Isabelle and pating in experiments involving the Verner have shown for their chosen PULSTAR reactor’s core. field ought to be cause for hope if not “It just gets cooler and cooler,” she said. celebration, and the support they’ve gotten from their NSUF mentor, For Verner, the internship this summer Brenden Heidrich, has greatly rein- has been a natural extension of the forced their determination to pursue work she has been doing at the Center careers in nuclear energy. for Advanced Energy Studies, where the NSUF has its offices. A native of “I believe nuclear power will be an Idaho Falls with a master’s in essential component in the future energy production of the United States

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biological engineering, she is now stored until their radioactivity levels changing the locations of sample pursuing a doctorate in nuclear engi- are low enough for examination,” she irradiation tubes,” she said. The neering from UI. She has also become said. “The purpose of my project was availability of a central irradiation a key member of Students for Nuclear to design a radioactivity calculator, experiment location, within the NC (http://www.students4nuclear.org/), which will estimate the radioactivity State reactor has shown a threefold a nationwide advocacy group. levels of materials post-irradiation. The increase in neutron flux exposure for calculator is intended to be an easily experiment samples. This should be a All three interns’ work has involved accessible tool for NSUF researchers benefit to PULSTAR, especially where computer simulations. Verner focused during the conceptual design phase of it relates to the effects of increased on a neutron damage calculator aimed their experiments.” fuel enrichment. at helping researchers determine which NSUF research reactor is best Making it easier to estimate the radio- “Interns always have new ideas and suited to the kind of research they activity of a sample before it is ever new ways of looking at things,” want to do. This involves modeling irradiated will have three benefits, she Heidrich said. “I like to think I’m flex- the reactor, calculating the amount said: increased worker safety aware- ible, but I’ve been at this awhile. I have of damage incurred by a number of ness, improved efficiency by planning to rethink a lot of things when I have material options in different experi- the examination work at the appro- to re-explain them. Sometimes, we get mental reactor positions, and building priate facility, and information that results we don’t expect.” a tool that will be on the NSUF will allow researchers to plan project He credited all three as “total self- website for users to access. timelines efficiently due to a better starters,” which is a benefit for intern understanding of required decay time. Holden’s project has been a radioac- research projects. Isabelle’s research tivity calculator to estimate the radio- Both Holden and Verner say the NSUF’s ought to be invaluable to NC State activity levels of materials post-irradi- material library and research database and the PULSTAR. “All three projects ation. “Materials with short half-lives has been essential to their work. “They involved developing tools to help are able to decay prior to the sample have access to many of the reactor researchers design better experiments, being removed from the reactor. simulation models,” said Verner. which is what the NSUF is all about,” Materials with longer half-lives must said Heidrich. Verner and Holden, Isabelle said what the NSUF has made be handled with caution and often who are staying in Idaho Falls to available to her relates directly to the pursue their degrees, will have time to peripheral experiments she did at NC finish up their NSUF projects. State. “My objective was to analyze whether experimental flexibility As for having three women for could be improved by increasing or protégés, Heidrich said it was “just kind of how it fell out. There were a lot of applicants. These three were the best fit for the NSUF.”

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Kelly Verner, NSUF Intern, and J. Rory Kennedy, NSUF Director, at the Summer 2017 INL Intern Poster Session. (Chris Morgan, INL)35 Nuclear Science User Facilities

FOCUS ON RESEARCH

Dr. Peter Hosemann Dr. Peter Hosemann values exchange of capabilities, ideas through the NSUF

r. Peter Hosemann of the conducting research on ion beam irra- University of California, diations and microscale mechanical DBerkeley Nuclear Engineering testing as well as liquid metal corro- (UCBNE) is the latest chairman of sion at Los Alamos National Labora- the Nuclear Science User Facilities tory (LANL). (NSUF) Users Organization. Elected Hosemann’s interest in materials and in November 2017, he acts as liaison radiation began as an undergraduate between NSUF users and facilities and in Switzerland and got into full swing NSUF management. Part of the NSUF in 2003, when he spent a summer partnership since 2011, UCBNE assists studying at LANL. In the Materials nuclear material scientists by making Science in Radiation and Dynamics the institution’s materials equipment Extremes group, he developed an available to interested researchers. interest in how materials respond in Hosemann’s enthusiasm for the extreme environments. “Radiation benefits of the NSUF drove his interest adds essentially another dimension, in the Users Organization. “The another axis on your diagram,” he NSUF is a genius idea,” he said. “By said. “You tackle problems that don’t connecting new researchers with exist anywhere else. It was different new ideas with the necessary partner and more interesting than anything I’d facilities, the NSUF also raises intellec- ever encountered.” tual nuclear science capital across the He returned to LANL as a graduate research community.” student in 2005 – a lot of people at Hosemann joined the Berkeley faculty LANL call New Mexico the “Land of in 2010 as assistant professor and was Entrapment,” he joked – and became promoted to associate professor in a postdoc in 2008. “The variety of 2014. He is department co-chair, head expertise available was considerable,” graduate adviser, and UC Berkeley’s he said. “You could approach almost radiation safety committee chair. He anyone for help and advice and they’d received his doctorate in material be willing to give it. I also appreciated science from the Montanuniversität the fact that my ideas were treated as Leoben, Austria, in 2008, while equal to anyone else’s. Being young or a student didn’t matter as long as the idea and science was sound.”

36 2017 | ANNUAL REPORT

Researcher Peter Hosemann, Nuclear Materials Laboratory, University of California, Berkeley (UCB) (Courtesy of UCB)37 Nuclear Science User Facilities

Researcher Peter Hosemann, Nuclear Materials Laboratory, University of California,38 Berkeley (UCB) (Courtesy of UCB) 2017 | ANNUAL REPORT

After getting his doctorate that year, • Liquid metal corrosion of structural he continued his research at LANL, materials for nuclear applications. focusing on structural materials This involves a fundamental under- used for nuclear components and standing of mechanisms that lead developing a basic understanding of to improved alloying concepts and degradation processes in a nuclear system operating techniques, with environment. He worked extensively the overall goal of reducing corro- in the Ion Beam Materials Laboratory sion issues. at Los Alamos, crediting the people Since 2008, Hosemann has authored and the lab’s overall culture with the more than 130 peer-reviewed articles. “The NSUF is a genius idea,” outlook he brought to Berkeley. In 2014, he was named best reviewer Under Hosemann’s leadership, UCBNE by the Journal of Nuclear Materials and he said. “By connecting new continues to develop new tools and also received the American Nuclear techniques as part of the NSUF system. Society’s literature award. In 2015, researchers with new ideas Hosemann welcomes researchers who he won the The Minerals, Metals and find uses for UCBNE capabilities that he Materials Society (TMS) Early Career might not have considered. Faculty Fellow Award and The American with the necessary partner Institute of Mining, Metallurgical, and “Truly, everybody who wants to use Petroleum Engineers (AIME) Robert it can. The NSUF gets you engaged in Lansing Hardy Award. facilities, the NSUF also other areas and broadens everyone’s horizons in the nuclear community. Hosemann also leads the UCB This was paid for by taxpayers, and to Bladesmithing team, which won the raises intellectual nuclear get the best use of taxpayer money, the title of “best example of a traditional tools and techniques developed should blade” for UCB, and is the lead science capital across the be available. What we are doing needs faculty member for the CalSol solar to be relevant to the broader DOE car racing team, which won the nuclear community.” American Solar challenge for Berkeley research community.” in 2017. His current research focus can be broken down into three parts: As for the NSUF Users Organization, Hosemann intends to • Small-scale materials testing on expand communications among users irradiated and unirradiated structural through improved use of the Users materials. This is aimed at reducing Organization website, hosted by the the necessary sample volume to a NSUF at nsuf.inl.gov, and through minimum in order to assess the the NSUF Users Organization email materials state while investigating distribution list. the basic effects of radiation damage. • New advanced structural materials concepts (e.g., oxide dispersion- strengthened steels) for nuclear applications using accelerated materials testing via ion beam irradiations.

39 Nuclear Science User Facilities

Riley Parrish The NSUF launches a research career

n the evolution of any Parrish said the more he learns about organization, institutional memory nuclear materials and fuels, the more Iand continuity are key to long- fascinating he finds them. While most term success. As the Nuclear Science materials involve looking at only one or User Facilities (NSUF) passes its tenth two major stimuli – high temperatures, anniversary, some of the people who corrosion, mechanical strength, stability were “present at the creation” in – all of these considerations must be support roles have become the leaders. accounted for in a reactor environment. University of Florida graduate student “It’s a complex puzzle that has been Riley Parrish freely concedes that studied for decades now, but we’re still without the resources of the Nuclear actively learning about the intricacies Science User Facilities he would not of what happens to the fuel in such a have been able to accomplish what he hostile environment,” he said. “It binds has since the beginning of 2017. so many materials disciplines together to work toward a singular goal of safe With NSUF funding and resources, and efficient fuel performance.” he has completed multiple Rapid Turnaround Experiments focused on MOX fuels will be an important cog three-dimensional microstructural and in the process of closing the nuclear chemical characterization of mixed fuel cycle, he said. They can incorpo- oxide (MOX) fuels at varying stages of rate plutonium from spent nuclear burnup. The funding would not likely fuel and decommissioned nuclear have been available from any other weapons to eliminate dangerous long source, and the resources definitely half-life elements from storage and would not have been. “The NSUF promote nonproliferation. was able to provide access to unique “Nuclear fuel reprocessing will be capabilities compared to universities critical to the success of limiting the and has been a great benefit to my potential environment impacts associ- research area,” Parrish said. ated with spent nuclear fuel, and MOX After completing his undergraduate fuels are just one form of fuel we can degree at Boise State University in use to make sure that the energy is 2015, Parrish spent two summers produced as efficiently as possible,” at INL working on energy storage he said. “My work is looking to study systems in the Summer Under- the fuel as it evolves in the reactor, to graduate Laboratory Internship extend the lifetime of the fuel in a safe (SULI) program. He joined Dr. Assel and effective manner.” Aitkaliyeva at the University of Florida Parrish’s Rapid Turnaround Experi- in spring 2017 and has traveled back ments have been sequential, exam- to Idaho on multiple occasions to ining MOX fuel specimens that were conduct his work at INL’s Materials & first irradiated in the mid-1980s as Fuels Complex. part of a core demonstration

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Riley Parrish, University of Florida, using the Focused Ion Beam (FIB), the Electron Microscopy Laboratory (EML), MFC, INL (Chris Morgan, INL) 41 Nuclear Science User Facilities

Riley Parrish, University of Florida, using the FIB, EML, MFC, INL 42 (Chris Morgan, INL) 2017 | ANNUAL REPORT

experiment at the Fast Flux Test between the University of Florida, Facility, located at DOE’s Hanford home to the Nuclear Fuels and Mate- Site. Taking advantage of the sophis- rials Characterization Facility, an NSUF ticated characterization tools needed partner facility, and INL. to understand fuel chemical and Parrish was on the cover of the structural characteristics, he has been February 2018 edition of Nuclear “The NSUF was able to conducting detailed microstructural News, which featured a special section examination of the prototypic fast on NSUF capabilities. A native of reactor fuel pins. The specific focus provide access to unique south-central Idaho, he enjoys biking, is on the ACO-3 fuel subassembly, backpacking, and climbing. He admits which achieved a peak burnup of that he is still adjusting to what capabilities compared to ~21 percent. The fuel pins had been Florida has to offer. previously sectioned and stored in the Materials and Fuels Complex’s Hot Beyond graduation, Parrish believes universities and has been a Fuel Examination Facility (HFEF). environmental conservation will be the greatest challenge to the world in Fuel pins are being thoroughly great benefit to my research the next 50 years, and he is passionate examined using scanning electron about clean energy advocacy and microscopy (SEM) to both characterize advancement. “I believe that new area,” Parrish said. the fuel microstructure and identify nuclear reactor technologies will need regions of interest for lamella and block to play a significant role in the future extraction. A radial approach is being energy landscape and I would love used to create tomography blocks to contribute to the promotion of and transmission electron microscopy the science, whether that is through lamella aimed at helping understand the active research at one of the national effects of irradiation conditions on the labs or through policy and public local microstructures of the fuel pellets. communications, to promote oppor- Microstructural and microchemical tunities for advancement in the U.S.,” examination of the prepared samples he said. “Nuclear energy has never had provides insight into the effects of radial a technology problem. It has always position in the fuel pellet on structure been a perception problem and I and composition of the samples. believe public outreach and activism is INL’s Focused Ion Beam (FIB) tool is the best way to brighten the future of being used to prepare tomography nuclear energy production.” blocks, which are then stored on site at INL for future use. Parrish estimated his time will be split roughly 60-40

43 Nuclear Science User Facilities

Luca Capriotti Introducing NSUF Instrument Scientists

uca Capriotti, NSUF Instrument point behavior of oxide materials. Scientist, always knew he wanted His research involved quite of bit of Lto work and conduct research glovebox work (more on that later!). in the United States. “The nuclear Capriotti’s research activities intro- industry is more developed and the duced him to several NSUF and INL national laboratory system offers great scientists and leaders, including NSUF research and professional development Director Rory Kennedy and HFEF opportunities,” he explained. Director Heather Chichester. His Ph.D. Capriotti is fully qualified on the research project started in 2013 and Physical Properties Measurement was on post irradiation examination System (PPMS), which will be of metallic fuel with minor actinides. installed and up and running in INL’s Six months before the end of his Ph.D. Irradiated Materials Characterization work at the European commission, he Laboratory (IMCL) by Summer 2018 began to scan the INL career website for radioactive materials. A second on a regular basis and successfully instrument is also available in the INL applied for his current position in July Research Center for cold samples and 2015. Since then, time has flown by. “I like talking about new depleted uranium. “When friends and family ask how Growing up in San Benedetto del I am, I always say that I’m living the Tronto, a town on Italy’s east coast, projects and areas of research, dream,” said Capriotti. In addition to Capriotti knew that he wanted to work his NSUF research, he works on the in the applied sciences. After high Advanced Fuel Campaign, concen- and I can work with you on school, he moved to Milan and earned trating on post irradiation examina- his Bachelor’s and Master’s degrees in tion (PIE) activities for Dr. Jason energy engineering. project feasibility.” Harp. He is one of two scientists fully Nuclear sparked his interest early on. qualified on the PPMS, along with INL “Nuclear physics had more depth scientist Krystoff Goffryk, who is the and interest to me than mechanical scientific supervisor. engineering,” he said. “The nuclear His request to NSUF researchers inter- engineering department was a great ested in how they can use the PPMS in learning environment. It was a small their work is straightforward: “Please department and we were like a family.” call or email me. I like talking about Nuclear engineering also provided new projects and areas of research, an opportunity for experimental and I can work with you on project research, which captivated him. Capri- feasibility. The earlier, the better, otti knew this was his calling. In 2011, since we can discuss approaches and he moved to Karlsruhe, Germany, to timing considerations, which can work with the European Commission then be incorporated into your NSUF on his graduate project: laser tech- proposal.” niques for high temperature melting

44 2017 | ANNUAL REPORT

Luca Capriotti, NSUF Instrument Scientist, using a shielded FEI Helios plasma focused ion beam instrument, Irradiated Materials Characterization Laboratory (IMCL), MFC, INL (Chris Morgan, INL) 45 Nuclear Science User Facilities

Fidelma Di Lemma, NSUF Instrument Scientist, using a Scanning Electron Microscope (SEM), 46 FASB, MFC, INL (Chris Morgan, INL) 2017 | ANNUAL REPORT

Fidelma Di Lemma Fidelma Di Lemma pursues the urgency of doing

idelma Di Lemma was born A fateful decision in high school an inventor with a passion for broadened Di Lemma’s career options Fadventure. “My father is an to include engineering. For her grad- engineer and many of my family uation project, she decided to focus members are in engineering, so I on the petrol crisis in the 1970s. Di wanted to try something new and Lemma became absorbed by how the unexpected,” she explained. Her world would meet growing energy journey to joining the NSUF as an demands moving forward. “I always instrument scientist spans the globe took mathematics and science classes. and encompasses her novel approach I’m adept in mathematics and enjoy to the sciences and engineering. both disciplines.” Growing up in a small Italian village Her fascination with novel and outside of Rome, Italy, she had innovative approaches has also ready access to world-renowned shaped her approach to engi- art history for inspiration, as well neering. “Nuclear engineering as a treasure trove of toys (and added an additional dimension and the occasional appliance) that she complexity to electricity genera- relished disassembling. “As a kid I tion beyond the need to turn a would break things to see how they turbine, Di Lemma said. “I became would work,” she said. With an Irish more interested in nuclear science mother and an Italian father, travel and engineering than in electricity was a way of life — a familiarity that production, per se.” She pursued a would serve her well as an adult. B.S. in energy engineering, followed She grew up bilingual in English by an M.S. in nuclear engineering. and Italian and learned additional languages through travel.

47 Nuclear Science User Facilities

Leonardo da Vinci said, “I have for fresh fuel, which will soon be been impressed with the urgency moved from INL’s Fuels and Applied “Please contact me if you of doing. Knowing is not enough; Sciences Building (FASB) to INL’s we must apply. Being willing is not Irradiated Materials Characteriza- are writing a proposal. I like enough; we must do.” Always inter- tion Laboratory (IMCL), and the ested in the practice as much as the electron probe microscope (EPMA) theory, Di Lemma enthusiastically for irradiated materials, located in to talk with researchers as began her research at the European the IMCL. She is fully qualified on Commission Joint Research Labora- the SEM and partially qualified on tory in Karlsruhe, Germany. Her the EPMA. they’re developing a proposal. Ph.D. research focused on using Di Lemma is also working to develop laser heating techniques for aerosol techniques for sample preparation production to simulate radiation I can help with scheduling for electron backscatter diffraction dispersal devices, which required (EBSD) research. The techniques frequent use of a glovebox for permit the determination of grain and feasibility and make life research. The story of the glovebox size and orientation, and to inves- begins on page 50. tigate stress and deformation in easier for everyone involved Di Lemma joined INL in 2016, materials and require keeping current following a post-doc stint in Tokai- in new research approaches as well as with the project.” mura, Muramatsu, Japan, with the a sound basis in current practices. Japan Atomic Energy Agency. “I liked What advice does she have for my work and coworkers in Japan, researchers interested in using but my life was calling to me to INL capabilities? Idaho,” she said. Her staff position put her in place to become fully “Please contact me if you are writing a qualified for two instruments: the proposal. I like to talk with researchers scanning electron microscope (SEM) as they’re developing a proposal. I can help with scheduling and feasibility and make life easier for everyone involved with the project.”

48 2017 | ANNUAL REPORT

Fidelma Di Lemma, NSUF Instrument Scientist, using an SEM, Fuels and Applied Sciences Building, MFC, INL (Chris Morgan, INL) 49 Nuclear Science User Facilities

THE GLOVEBOX

A Tale of Actinides and Love

uca Capriotti and Fidelma Di Talking over their respective work Lemma met while working soon led to discussions about their Lside-by-side with adjoining respective lives and backgrounds and gloveboxes at the Institute for future plans and dreams. Italian is a Transuranium Elements in Karlsruhe, romance language, which no doubt Germany. Their respective work both helped. A shared interest in under- focused on decoding the magic of standing nuclear energy needs and nuclear science – more specifically, barriers across the globe created their the behavior of actinide materials first joint venture: participation in subjected to high temperatures. international organizations of nuclear professionals, including the Interna- Actinides are any of the series of tional Youth Nuclear Congress. fifteen metallic elements from actinium (atomic number 89) to “I wanted to be better connected to lawrencium (atomic number 103) in the nuclear industry and understand the periodic table. They are all radio- nuclear research needs in Germany active, the heavier members being and around the world,” said Capriotti. unstable and human-made. Although His research landed him opportuni- quite interesting to nuclear scien- ties with the European Space Agency tists and engineers who are always in Madrid, Spain; Ph.D. studies at the seeking improvements in nuclear Technische Universität München in fuels, actinides do not typically fill Munich, Germany; and the European the dreams of little boys and girls Commission Joint Research Centre in imagining the great romance that will Eggenstein-Leopoldshafen, Germany. signal the arrival of their life partner. Meanwhile, the Institute for Trans- What stray atomic attraction brought uranium Elements asked Di Lemma Capriotti and Di Lemma together? to stay to commence a contract as a Ph.D student. She then started a new “We were working side by side post doctoral research fellow posi- and we’re both Italian,” explains Di tion with the Japan Atomic Energy Lemma, laughing. “It would have been in Muramatsu, Japan, while Capriotti more strange if we hadn’t met.” remained in Germany.

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Luca Capriotti and Fidelma Di Lemma, IMCL, MFC, INL (Chris Morgan, INL) 51 Nuclear Science User Facilities

Luca Capriotti and Fidelma Di Lemma at the HFEF, MFC, INL. Capriotti is using a new inverted optical microscope (Leica model DMi8, modified for hot cell settings). (Chris Morgan, INL) 52 2017 | ANNUAL REPORT

“We were both in International Youth “The global function of IYNC provides Nuclear Congress (IYNC) leadership members with a better understanding positions,” said Di Lemma. “Sometimes of the nuclear communities around the IYNC meetings were the only times the world,” said Di Lemma. “In terms we were in the same country.” of managing teams, I’ve learned to be clear with what the “ask” is and the They became engaged in March 2015 timeline necessary to meet commit- just before Di Lemma went to Japan. ment – and to give participants a Capriotti was first to join INL in early way to opt out if necessary, as we are 2016. Di Lemma accepted a position volunteers dedicating whatever time with INL in late 2016. They married we can find.” June 2017 in Rome, Italy. What’s next in store for this Involvement in the IYNC does not research duo? guarantee marriage for everyone, although Di Lemma says that she “I’m enjoying becoming certified knows of another happily married on the electron probe microscope couple who met through the orga- (EPMA) for irradiated materials,” said nization. Capriotti and Di Lemma Di Lemma. “The opportunities the maintain their strong participation NSUF has provided, like presenting for professional reasons. In fact, my research at the annual program Capriotti was elected in March 2018 review, are giving me a valuable to a two-year term as IYNC President perspective on how a successful at a biennial conference. At the same research program operates.” conference, Di Lemma managed As for Capriotti? “I'm already living the first-ever session of the IYNC the dream,” he said with a smile. “I International Innovation Congress have the opportunity for research and I4N (Innovation for Nuclear), which professional development. I’m happy.” saw teams from all over the world proposing innovative solution to the challenges facing the nuclear industry. “IYNC fosters leadership skills, especially in coordinating the efforts of a team,” said Capriotti. “Involvement helped me to gain a broad perspective on culture and learn protocols for business.”

53 Nuclear Science User Facilities

NEW NSUF PARTNERSHIPS

XPD Beamline, NSLS-II, Brookhaven he Nuclear Science Users Partner Facilities National Laboratory Facility (NSUF), a network of Tnuclear energy research institu- Added in FY 2017 tions across the United States, added Brookhaven seven new partner facilities in FY National Laboratory 2017 and one international affiliate. National Synchrotron Light Source II While ATR – the only materials test Core Functions: X-ray beams. reactor in the United States that can Brookhaven National Laboratory’s replicate multiple reactor environ- NSLS-II enables the study of mate- ments concurrently – remains the rial properties and functions with crown jewel, the NSUF has expanded nanoscale resolution and exquisite its scope over ten years to incorporate sensitivity by providing world-leading a wide variety of reactor and research capabilities for X-ray imaging and facilities from coast to coast. high-resolution energy analysis. The NSLS-II is a medium energy (3.0 GeV) electron storage ring designed to deliver photons with high average spectral brightness exceeding 1021 ph/s in the 2–10 keV energy range and a flux density exceeding 1015 ph/s in all spectral ranges.

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Lawrence Livermore National Laboratory Center for Accelerator Mass Spectrometry Core Functions: Accelerator ion irradiation, ion beam analysis and mass spectroscopy. CAMS hosts a 10-MV FN tandem Van de Graaff accelerator, a NEC 1-MV tandem accelerator, and a soon to be commissioned 250KV single stage accelerator mass spectrometry (AMS) deck will perform up to 25,000 AMS measurement per year. The Center also has an NEC 1.7-MV tandem accelrator for ion beam analysis and microscopy. The research and development made possible by AMS and ion beam analytical techniques is diverse and includes material analysis and modification studies, as well as nuclear The research team at the Center for Accelerator Mass Spectrometry (CAMS), physics cross-section measurements Lawrence Livermore National Laboratory (LLNL) (Courtesy of LLNL). and nuclear chemistry studies. Los Alamos National Laboratory Lujan Center at Los Alamos Neutron Science Center (LANS) Core Functions: Cold neutron scattering and diffraction techniques. The LANS features instruments that operate in time-of-flight mode, receiving neutrons from a tungsten spallation target. Four modera- tors provide epi-thermal, thermal and cold neutrons to specialized beamlines. The available instrument suite includes the Spectrometer for Materials Research at Temperature and Stress (SMARTS); High-Pressure- Preferred Orientation instrument (HIPPO); Flight Path 5 for energy- resolved neutron imagining; and other beamlines, as available. Researchers preparing for an experiment on the High Pressure Preferred Orientation (HIPPO) Instrument in the Lujan Center at the Los Alamos Neutron Science Center (LANS), Los Alamos National Laboratory (LANL) (Courtesy of LANL).

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Wing 9 Hot Cells Plutonium Surface Core functions: remote testing. Science Laboratory Core Functions: Oxide Fuel Fabrication The Los Alamos National Laboratory (PuO ) and characterization. Wing 9 Hot Cells consist of four 2 shielded cells for mechanical testing The Plutonium Surface Science (including tension, compression, bend Laboratory provides capabilities in bar, ring pull and harness testing); scanning tunneling microscopy and machining/cutting/polishing; sample spectroscopy, atomic force microscopy, handling and storage; cleaning; and infrared reflection-absorption spec- shipping and receiving. Support troscopy, secondary ion mass spectros- equipment includes a 10-ton crane copy, x-ray and ultraviolet photoemis- for interior sample movement and sion spectroscapies, profilometer, and a 25-ton crane for equipment. The gas chromatograph mass spectroscopy. Wing 9 Hot Cells accept beta-gamma materials only.

The Ohio State University The Ohio State University Nuclear Reactor Laboratory (OSU-NRL) Core Functions: Thermal neutron irradiation of nuclear fuels and materials and instrumentation. The OSU-NRL offers the unique capability of reactor irradiations in external large-volume experiment dry tubes at temperatures from 4 K to 1873 K. Uses include experiments involving instrumented, high- temperature irradiations of prototype instrumentation for next generation reactors, sensors, and sensor materials, as well as optical fibers designed for up to 1600°C.

View from the top of the pool at the Ohio State University Research Reactor, The Ohio State University (Courtesy of The Ohio State University)

56 2017 | ANNUAL REPORT

Researcher Khalid Hattar using the In Situ Ion Irradiation Transmission Electron Microscope (I3TEM) in the Ion Beam Laboratory, Sandia National Laboratories (Courtesy of SNL).

Sandia National Laboratories Gamma Irradiation Facility (GIF) Annular Core Research Ion Beam Laboratory (SIBL) Core Functions: Gamma irradiation of Reactor (ACRR) Core Functions: Ion irradiation, ion beam materials and sensors using Co-60 sources. Core Functions: Safety testing of modification, ion beam analysis and high nuclear fuel samples and instrumentation. The GIF produces a wide range of magnification imaging. gamma radiation environments using The ACRR is an epi-thermal pool- The In Situ Ion Irradiation Transmis- Co-60 sources. The GIF is capable of type reactor which uses cylindrical sion Electron Microscope (I3TEM) irradiating objects as small as bacteria UO2-BeO fuel elements. Researchers Facility at the SIBL offers ion irradia- and as large as an Abrams M1 tank perform sample irradiations in typical tion, including in situ irradiation in a (although SNL typically irradiate research reactor steady-state mode or TEM with specialty specimen stages electronic components, equipment in a high-power pulse mode, reaching available, such as heating, cooling, and samples of various materials). The powers as high as 30GW strain, compression, and changes in GIF provides in-cell dry irradiations for a few milliseconds. There are specimen environment. The I3TEM in test cells and in-pool submerged four main experimental cavities at the Facility offers the capabilities of a irradiations in the pool. The GIF has ACRR facility: central cavity, FREC-II 200 kV JEOL 2100 high-contrast TEM three concrete dry test cells: two cells cavity, thermal neutron beam tube combined with the implantation/ are 3 m × 3 m, one cell is 5.5 m × (the neutron radiography facility), irradiation capabilities of the 9.1 m, and an 18-foot deep pool. The and the Tri-Element facility. The ACRR 10 kV Colutron and the 6 MV Tandem facility offers gamma dose rates from is complementary to TREAT (INL), accelerators housed in the SIBL. SIBL’s 10-3 rad/s to over 1000 rad/s. focusing more on electronics eight accelerators cover a wide range testing for the National Nuclear of energies and ions. Security Administration.

57 Nuclear Science User Facilities

Researchers in the Texas A&M Accelerator Laboratory, Texas A&M University (Courtesy of Texas A&M University).

Texas A&M University a 10 kV ion accelerator (with a gas a 1.7 MV Ionex Tandetron Accelerator Texas A&M Accelerator Laboratory ion source); a 150 kV Ion Accelerator (with an RF plasma source and a Core Functions: Ion irradiation and (with a universal ion source); a 200 SNICS source); a high temperature ion beam analysis. kV ion accelerator (with a universal vacuum furnace; a high temperature ion source); a 1 MV Ionex Tandetron gas furnace; a four-point-probe The Texas A&M Accelerator Labora- Accelerator (with a RF plasma source resistivity measurement; and various tory is one of the largest university and a Source of Negative Ions by heating and cooling systems for ion ion irradiation facilities in the United Cesium Sputtering (SNICS) source); irradiations at different temperatures. States. Key facilities in the lab include:

University of Florida Nuclear Fuels and Materials Characterization Facility (NFMC) Core Functions: Materials characterization of irradiated materials. The NFMC provides capabilities in microstructural characterization and mechanical properties evaluation of materials-related research with an emphasis on nuclear. The laboratory is dedicated to supporting radiological work and the University of Florida Teaching Reactor.

Dual Beam Focused Ion Beam (FIB) and Scanning Electron Microscope (SEM) at the Nuclear Fuels and Materials Characterization Facility, University of Florida (Courtesy of University of Florida).

58 2017 | ANNUAL REPORT

International Affiliate Added in 2017 SCK•CEN Belgian Reactor 2 (BR2) Core Functions: Advanced fuel and materials irradiation. Versatile core configurations. BR2 is among the most powerful and flexible research reactors in the world. BR2 irradiates all kinds of nuclear fuels and materials for different types of reactors and the European nuclear fusion program. The intense radiation allows researchers to study aging of irradiated materials. The core can be reconfigured to accommodate custom experimental items. Laboratory for High and Medium Activity (LHMA) Core Functions: Materials characterization of highly irradiated materials. The LHMA focuses on the effects of radiation on materials, such as in the pressure vessels of nuclear reactors or the effects of uranium fission in the reactor fuel. The laboratory has the necessary infrastructure to handle highly radioactive substances safely. The study of fuel pins from reactors around the world is supported.

View of the reactor core of the Belgian Reactor 2 (BR2), SCK•CEN.

59 Nuclear Science User Facilities

NSUF-GAIN SYNERGY Synergy of the NSUF with the DOE GAIN Initiative

he Gateway for Accelerated from the nuclear industry as well as Innovation in Nuclear (GAIN) those from universities, government Tinitiative was established to laboratories, and small businesses. The address issues that constrain innova- GAIN initiative and the NSUF program tion in the domestic nuclear industry. thus represent a powerful combination As such, GAIN influences the direc- of resources for those contributing tion and priorities of relevant U.S. to re-establishing the U.S. leadership Department of Energy, Office of position in nuclear power. Nuclear Energy (DOE-NE) research, In principle, the advanced and development and deployment innovative fuels and materials vetted J. Rory Kennedy (RD&D) programs and functions as a through NSUF experimental research Director framework for private-public partner- would be picked up by GAIN and (208) 526-5522 ships. The GAIN initiative offers a its network of industry members to [email protected] single access point to a broad range move forward with commercializa- of expertise and capabilities over tion and deployment of these mate- many subject areas and promotes rials. The DOE-NE Memorandum of working relationships between Understanding with the U.S. Nuclear nuclear technology developers and Regulatory Commission (NRC) on DOE national laboratory expertise. implementation of GAIN is one tool The Nuclear Science User Facili- to apply here. The NSUF in 2017 ties (NSUF) program is focused on awarded industry-led Consolidated understanding irradiation effects in Innovative Nuclear Research (CINR) nuclear fuels and materials and, for this projects addressing the joining of particular subject area, is a key contrib- advanced SiC-SiC cladding to General utor to the GAIN initiative. The NSUF Atomics, advanced neutron absorbing offers the nuclear community access to materials to AREVA, an additive capabilities and expertise at the unique manufacturing process from Westing- facilities at Idaho National Labora- house, and two projects to Electric tory (INL) and 20 additional partner Power Research Institute (EPRI), one facilities. The nuclear community that on high burnup fuel and another on the NSUF supports includes researchers the hydrogen pickup mechanism in

60 2017 | ANNUAL REPORT

Zircaloy-2. These examples indicate will collaborate on additional work- how the NSUF operates at all shops to support the current fleet as Technology Readiness Levels in well as advanced reactor concepts. addressing specific scientific questions Examples that cover both areas would of interest to industry (See table). be potential workshops on Advanced Manufacturing and Advanced Beginning in 2017, the NSUF and Modeling and Simulation capabilities. GAIN began collaborating on industry The NSUF also regularly invites GAIN outreach workshops in order to to participate in its Industry Advisory maintain and improve (where neces- Committee meetings. sary) responsiveness to industry needs that the DOE-NE can address. The NSUF thermal hydraulics workshop FY 2017 Consolidated Innovative was held in cooperation with GAIN Nuclear Research (CINR) Awards to Industry in order to assess and prioritize thermal hydraulics facilities that might General Atomics Performance of SiC-SiC Cladding and Endplug contribute most to the mission of Joints Under Neutron Irradiation with a DOE-NE in advancing technologies, Thermal Gradient particularly for small modular reactor AREVA Irradiation of Advanced Neutron Absorbing designs. The NSUF recently included Material to Support Accident Tolerant Fuel a GAIN representative in its workshop to develop a Fuels and Materials Electric Power Irradiation, Transient Testing and Post Irradiation Understanding Scale (FaMUS) that Research Institute, Inc. Examination of Ultra High Burnup Fuel will provide a means to indicate the Westinghouse Radiation Effects on Zirconium Alloys state of understanding of the behavior Electric Company Produced by Powder Bed Fusion Additive of a particular material in reactor. Manufacturing Processes Implementation of this scale will Electric Power Improved Understanding of Zircaloy-2 aid in assessing the impact of NSUF Research Institute Hydrogen Pickup Mechanism in BWRs research on the nuclear industry in addressing questions of importance. Going forward, the NSUF and GAIN

61 Nuclear Science User Facilities

MEASURING IMPACT

Journal Publications

Conference Proceedings

0 2008 2009 2010 2011 2012 2013 2014 2015 2016 2017

2008 2009 2010 2011 2012 2013 2014 2015 2016 2017 Journal Publications 2 5 6 8 7 24 39 31 49 54 Conference Proceedings 1 2 11 6 12 31 27 27 34 41

Figure 1. NSUF Publications and Conference Proceedings by calendar year

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Researcher using the Local Electrode Atom Probe (LEAP), MaCS, CAES (Chris Morgan, INL)

A Peek Inside the NSUF NSUF Publications and Conference Proceedings

In order for the Nuclear Science The NSUF has tracked publications and User Facilities (NSUF) to fulfill conference proceedings since 2008, Ithe DOE-NE’s mission to advance and took additional steps in FY 2017 nuclear energy, NSUF researchers must to increase the number of self-reported publish and document research results publications and to improve the through peer-reviewed research jour- consistency in the data capture process nals and presentations at conferences. for collecting the lists of publications and conference proceedings.

63 Nuclear Science User Facilities

NSUF Experiment, Test Train Assembly Facility, ATR Complex, INL (Chris Morgan, INL)

Out of the 225 total publications for Expansion and Diversification the NSUF in 60 different journals, of the NSUF User Community 89 were published in the Journal of In order to evaluate how the NSUF is Nuclear Materials. This indicates that growing, several metrics are tracked NSUF projects are producing quality over time: scientific output and that the Journal of • the number of Rapid Turnaround Nuclear Materials is the most important Experiment (RTE) proposals journal to the NSUF nuclear community from a relevancy viewpoint. The • the number of RTE awards importance of this journal is also • the number of Consolidated emphasized by the fact that 26 of the Innovative Nuclear Research publications coming out of the NSUF (CINR) pre-applications were published in this journal in 2017. • the number of CINR full applications, and • the number of CINR awards

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180 35

170 RTE Proposals (2017 metric)

160 RTE Awards

150 29.4 29.4 30 *APS Proposals

140 *APS Awards

130 25 *Full/CINR Pre-Apps' 213

120 *Full/CINR Awards 22.2

110 New Budget Authority ($M) 20.4 100 20

90 17.7

Proposals/Awards 14.2 15 Budget in Millions 70 13.6 11.9 12.6 60

50 10

40 7.6

30 5 20

0 0 2008 2009 2010 2011 2012 2013 2014 2015 2016 2017

2008 2009 2010 2011 2012 2013 2014 2015 2016 2017 *APS Proposals 4 6 5 4 4 *APS Awards 4 2 1 1 3 RTE Proposals 8 10 25 27 35 49 76 180 RTE Awards 3 10 10 19 25 30 39 92 *Full/CINR Pre-Apps 20 29 15 8 9 7 4 31 67 108 *Full/CINR Awards 6 6 8 1 5 13 15 New Budget Authority ($M) 7.6 11.9 22.2 20.4 13.6 14.2 12.6 17.7 29.4 29.4 * Full/APS Awards transitioned to CINR Award in 2015

Figure 2. NSUF Proposals, Awards, New Budget Authority ($M)

65 Nuclear Science User Facilities

75 International Awards

National Lab Awards 70

University Awards 65

Industry Awards 60

Total PIs per year 213 55

New PIs per year 50

Minority-Serving Institutions (MSI) 45

35 Number of Awards

0 2008 2009 2010 2011 2012 2013 2014 2015 2016 2017

2008 2009 2010 2011 2012 2013 2014 2015 2016 2017 International Awards 0 0 0 0 0 0 0 3 3 6 National Lab Awards 0 0 3 2 2 3 13 12 20 36 University Awards 6 6 12 10 10 17 15 20 28 55 Industry Awards 0 0 0 0 0 0 0 0 1 10 Total PIs per year 6 6 15 11 11 15 20 24 42 78 New PIs per year 0 6 14 8 6 7 7 15 31 55 Minority-Serving Institutions (MSI) 2 1 1 1 1 0 3 6 4 0 FY 17 Data was analyzed against the UNITED STATES DEPARTMENT OF EDUCATION ACCREDITED POSTSECONDARY MINORITY INSTITUTIONS List: https://www2.ed.gov/about/offices/list/ocr/edlite-minorityinst-list-tab.html

Figure 3. NSUF Expansion and Diversification

66 2017 | ANNUAL REPORT

Quality Assurance inspection of upper locking mechanisms of reactor vessel surveillance capsules, Westinghouse Churchill Site (Courtesy of Westinghouse Electric Company).

To help evaluate expansion and diver- Gateway for Accelerated Innovation Proposal submissions to the NSUF have sification, the NSUF tracks the number in Nuclear (GAIN) initiative. GAIN grown at a rate that is outpacing avail- of combined CINR and RTE awards by is a DOE initiative that is focused on able funding. As a result, the awards year made to international, national addressing universally recognized have become more competitive. laboratory, industrial and university issues that currently constrain the institutions. A plot of the total number domestic nuclear industry. The NSUF of Principal Investigators (PIs) and new supports industry as follows: PIs per year is also tracked. • Provides federally funded experi- The NSUF continued its expansion mental data for all phases of the and diversification to international and innovation cycle industry requesters in FY 2017. NSUF • Maintains a database for critical research opportunities have received experimental facilities and equip- a significant increase in user interest ment that are of interest to GAIN from industry applicants. The increase participants in industry proposals demonstrates that • Develops and maintains the scientific industry regards NSUF as a viable asset. infrastructure through identified The increase in the industry usage equipment needs, measurement of the NSUF is due in part to the technique development and associ- NSUF’s proactive engagement with the ated expertise.

67 Nuclear Science User Facilities

AWARDED PROJECTS

he NSUF offers rapid turn- of NSUF’s capabilities at INL, the and over its distributed network of around experiments (RTEs) Microscopy and Characterization partner facilities. The tables of Tthree times per year. DOE in Suite (MaCS) at the Center for FY 2017 awards for the three calls FY 2017 awarded a total of Advanced Energy Studies (CAES), for RTE proposals are below. 94 RTE projects that will make use

FY 2017 First Rapid Turnaround Experiment (RTE) Awards (29)

PI Name Institution Title Facility Nathan University of Microstructural characterization of Oak Ridge National Laboratory – Low Almirall California Santa archival surveillance steels from the Activation Materials Development and Barbara Advanced Test Reactor (ATR-2) neutron Analysis (LAMDA) irradiation experiment Weiying Chen Argonne In situ Observation of Defect Clustering in Argonne National Laboratory – National High Entropy Alloys Intermediate Voltage Electron Microscope Laboratory Tandem Facility Yiren Chen Argonne Microstructural evolution of dual-phase Argonne National Laboratory – National cast stainless steels under irradiation Intermediate Voltage Electron Microscope Laboratory Tandem Facility Mahmut Oak Ridge Hydride microstructure at the metal- Oak Ridge National Laboratory – Low Cinbiz National oxide interface of Zircaloy-4 from H.B. Activation Materials Development and Laboratory Robinson Nuclear Reactor Analysis (LAMDA)

Philip Oak Ridge Microstructural and -chemical Oak Ridge National Laboratory – Low Edmonson National Investigations of the short-term annealing Activation Materials Development and Laboratory of irradiation-induced late blooming Analysis (LAMDA) phase precipitates in a high-Ni reactor pressure vessel steel weld David Frazer University of Localized mechanical property assessment University of California, Berkeley California, of neutron irradiated SiC/SiC composites Berkeley at elevated temperature

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PI Name Institution Title Facility Marine CEA Saclay Study of deformation mechanisms of Argonne National Laboratory – Gaumé zirconium alloys under irradiation Intermediate Voltage Electron Microscope Tandem Facility Jing Hu Argonne In situ ion irradiation and high resolution Argonne National Laboratory – National microstructure and microchemistry Intermediate Voltage Electron Microscope Laboratory analysis of accident tolerant fuels Tandem Facility Kookhyun University of Irradiation of the vanadium carbide University of Michigan – Michigan Ion Jeong Florida coating on HT-9 steel using protons Beam Laboratory Djamel North Carolina Ion beam radiation damage assessment Argonne National Laboratory – Kaoumi State University in advanced Ferritic/Martensitic Intermediate Voltage Electron Microscope (F/M) alloys Tandem Facility Jie Lian Rensselaer Radiation response and microstructure Center for Advanced Energy Studies

Polytechnic of accident tolerant U3Si2 fuels by ion – Microscopy and Characterization Institute beam irradiation Suite & Argonne National Laboratory – Intermediate Voltage Electron Microscope Tandem Facility

Jie Lian Rensselaer Micromechanical testing of sintered UO2 University of California, Berkeley Polytechnic fuel pellets with controlled microstructure Institute Yinbin Miao Argonne Fission gas bubble characterizations of Center for Advanced Energy Studies –

National high-energy Xe implanted U3Si2 Microscopy and Characterization Suite Laboratory

Yinbin Miao Argonne Xe bubble evolution in U3Si2: an in situ Argonne National Laboratory – National TEM Investigation Intermediate Voltage Electron Microscope Laboratory Tandem Facility

Arthur Motta Pennsylvania Cavity shrinkage in Fe21Cr32Ni under in situ Argonne National Laboratory – State University ion irradiation Intermediate Voltage Electron Microscope Tandem Facility Chad Parish Oak Ridge Microstructural recovery in irradiated Oak Ridge National Laboratory – Low National nanostructured ferritic alloys Activation Materials Development and Laboratory Analysis (LAMDA)

69 Nuclear Science User Facilities

PI Name Institution Title Facility Riley Parrish University of Microstructural characterization of 23% Idaho National Laboratory – Materials Florida burn-up MOX fuel and Fuels Complex Kumar University of Investigation of deformation mechanisms Oak Ridge National Laboratory – Low Sridharan Wisconsin - of an intermetallic-strengthened alloy Activation Materials Development and Madison with and without heavy ion irradiation Analysis (LAMDA) Cheng Sun Idaho National Characterization of ferritic steels Fe-9Cr and Center for Advanced Energy Studies – Laboratory 9Cr2WYT Oxide-Dispersion-Strengthened Microscopy and Characterization Suite (ODS) alloys irradiated in ATR Cheng Sun Idaho National The window of gas-bubble superlattice University of Michigan – Michigan Ion Laboratory formation in bcc metals Beam Laboratory Benjamin EPRI - Electric TEM investigation of irradiated austenitic Oak Ridge National Laboratory – Low Sutton Power Research stainless steel alloys Activation Materials Development and Institute Analysis (LAMDA) Elena Tajuelo Oak Ridge Changes on viscoelastic behavior, Oak Ridge National Laboratory – Low Rodriguez National morphology and chemical structure of Activation Materials Development and Laboratory gamma irradiated calcium silicate hydrates Analysis (LAMDA) with respect to nonirradiated samples Lizhen Tan Oak Ridge Radiation-hardening and Oak Ridge National Laboratory – Low National microstructural Stability of NF709 Activation Materials Development and Laboratory Austenitic Stainless Steel Analysis (LAMDA) Peter Wells University of Investigation of the thermal stability of Oak Ridge National Laboratory – Low California- Mn-Ni-Si precipitates in ion irradiated Activation Materials Development and Santa Barbara RPV steels Analysis (LAMDA) Haiming Idaho State Ion irradiation of advanced materials – University of Wisconsin – Tandem Wen University nanostructured steels and high Accelerator Ion Beam and the entropy alloys Characterization Laboratory for Irradiated Materials Yong Yang University of Low temperature Fe-ion irradiation University of Michigan – Michigan Ion Florida of 15-15Ti steel in different thermo- Beam Laboratory mechanical states Xinghang Purdue In situ studies of radiation damage in Argonne National Laboratory – Zhang University nanostructured austenitic stainless steels Intermediate Voltage Electron Microscope Tandem Facility

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Mock-Up Shop for new hot cell equipment, Fuel Conditioning Facility (FCF), MFC, INL (Chris Morgan, INL) 71 Nuclear Science User Facilities

FY 2017 Second Rapid Turnaround Experiment (RTE) Awards (30)

PI Name Institution Title Facility

Aida Michigan State Post-irradiation characterization of ion Oak Ridge National Laboratory – Low Amroussia University irradiation damage in Ti-6Al-4V and Activation Materials Development and CP-Ti : Influence of the microstructure Analysis (LAMDA) and temperature Alicia Raftery Purdue Pre-characterization of DISECT U-Mo fuel Center for Advanced Energy Studies – University samples Microscopy and Characterization Suite

Caleb Massey University Nano-precipitate response to neutron Center for Advanced Energy Studies – of Tennessee irradiation in model ODS FeCrAl Alloy Microscopy and Characterization Suite Knoxville 125YF

Cheng Sun Idaho National Nanoindentation testing of neutron Center for Advanced Energy Studies – Laboratory irradiated 304 stainless steels hex-blocks Microscopy and Characterization Suite

Chris Oxford In situ ion irradiation of second phase Argonne National Laboratory – Grovenor University particles in zirconium fuel cladding Intermediate Voltage Electron Microscope Tandem Facility Elena Tajuelo Oak Ridge Changes on viscoelastic behavior, Oak Ridge National Laboratory – Low Rodriguez National morphology and chemical structure Activation Materials Development and Laboratory of gamma irradiated calcium silicate Analysis (LAMDA) hydrates to 0.96MGy with respect to non-irradiated samples Elizabeth United States Radiation tolerance of friction stir Center for Advanced Energy Studies – Getto Naval Academy welded ferritic oxide dispersed steel Microscopy and Characterization Suite under ion irradiation Emmanuelle University of ά precipitation in neutron irradiated Oak Ridge National Laboratory – Low Marquis Michigan Fe-9/12Cr alloys Activation Materials Development and Analysis (LAMDA)

Gabriel Meric University of Sample preparation for ex situ TEM study Center for Advanced Energy Studies – de Bellefon Wisconsin - of deformation-induced twinning and Microscopy and Characterization Suite Madison martensite in two 316L austenitic stainless steels: role of stacking fault energy and grain orientation

Haiming Wen Idaho State APT study of neutron irradiated Center for Advanced Energy Studies – University U-Mo fuel Microscopy and Characterization Suite

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PI Name Institution Title Facility

Ian University of Enhancing radiation tolerance through Argonne National Laboratory – Robertson Wisconsin- increasing alloy complexity Intermediate Voltage Electron Microscope Madison Tandem Facility Jacqueline AREVA NP Inc. Hydrogen analysis and oxide Oak Ridge National Laboratory – Low Stevens characterization of reactor irradiated Activation Materials Development and Zr-Nb alloy Analysis (LAMDA)

Janelle Purdue Radiation induced segregation and Oak Ridge National Laboratory – Low Wharry University phase separation in neutron irradiated Activation Materials Development and FeCrAl alloys Analysis (LAMDA)

Jie Lian Rensselaer Fission gas behavior and fuel swelling of Argonne National Laboratory –

Polytechnic accident tolerant U3Si2 fuels by ion Intermediate Voltage Electron Microscope Institute beam irradiation Tandem Facility Jiming Bao University of Post irradiation examination of fiber Idaho National Laboratory – Materials Houston optic temperature sensors for in-pile and Fuels Complex temperature monitor and control for ATR

Jonathan Electric Power SEM, EBSD, and TEM investigation of Oak Ridge National Laboratory – Low Tatman Research irradiated austenitic stainless steel Activation Materials Development and Institute weldment Analysis (LAMDA)

Ju Li Massachusetts The in situ observation of radiation Argonne National Laboratory – Institute of resistance mechanism in metal-1D/2D Intermediate Voltage Electron Microscope Technology nanocomposites for structural material Tandem Facility and fuel cladding of next generation reactors Lingfeng He Idaho National Investigation of gas bubble behavior Argonne National Laboratory – Laboratory under ion irradiation Intermediate Voltage Electron Microscope Tandem Facility Mahmut Oak Ridge In situ TEM study of the ion irradiation Argonne National Laboratory – Cinbiz National damage on hydrides in a zirconium alloy Intermediate Voltage Electron Microscope Laboratory for nuclear fuel cladding Tandem Facility Ming Tang Los Alamos Radiation stability study on nuclear Argonne National Laboratory – National waste/spent fuel materials Intermediate Voltage Electron Microscope Laboratory Tandem Facility

73 Nuclear Science User Facilities

Experiment Sample, Materials Laboratory, CAES 74 (Chris Morgan, INL) 2017 | ANNUAL REPORT

PI Name Institution Title Facility

Mitra Taheri Drexel Quantitative assessment of the role of Argonne National Laboratory – University interfaces and grain boundaries in the Intermediate Voltage Electron Microscope development of radiation tolerant nuclear Tandem Facility materials Niels SCK•CEN Characterization of ion irradiated 15-15Ti Center for Advanced Energy Studies – Cautaerts steel by APT Microscopy and Characterization Suite

Osman El Los Alamos Performance of nanocrystalline and Argonne National Laboratory – Atwani National ultrafine Tungsten under irradiation Intermediate Voltage Electron Microscope Laboratory and mechanical extremes Tandem Facility Ramprashad Pacific Mechanical characterization of neutron Pacific Northwest National Laboratory – Prabhakaran Northwest irradiated FSW ODS alloys Radiochemistry Processing Laboratory National Laboratory Riley Parrish University of Microstructural characterization of 3% Idaho National Laboratory – Materials Florida burn-up MOX fuel and Fuels Complex Samuel A. Sandia National Study of nanocluster stability in neutron- Oak Ridge National Laboratory – Low Briggs Laboratories and ion-irradiated ODS FeCrAl alloys Activation Materials Development and Analysis (LAMDA)

Vijay University of Effect of grain boundary character and Center for Advanced Energy Studies – Vasudevan Cincinnati surface treatment on irradiation tolerance Microscopy and Characterization Suite of nuclear alloys Yutai Katoh Oak Ridge Micromechanical properties of interfacial University of California, Berkeley National elements in advanced SiC composite and Laboratory its environmentally protective coatings Zhangbo Li University of TEM investigation of radiation damage of Center for Advanced Energy Studies – Florida ferrite in CF-3 Microscopy and Characterization Suite

Zheng Zhang University of Pore size distribution in U-Mo fuel Idaho National Laboratory – Materials Florida irradiated to high burnup and Fuels Complex

75 Nuclear Science User Facilities

FY 2017 Third Rapid Turnaround Experiment (RTE) Awards (35)

PI Name Institution Title Facility

Adrien Couet University of Characterization of oxide layer on the Oak Ridge National Laboratory – Low Wisconsin surface of high temperature water Activation Materials Development and corroded Zircaloy-4 in the presence of Analysis (LAMDA) Neutron+Gamma and Gamma only Adrien Couet University of APT and TEM study of redistribution of Center for Advanced Energy Studies – Wisconsin alloying elements in ZrNb alloys following Microscopy and Characterization Suite proton irradiation: effects on in-reactor corrosion kinetics. Bei Ye Argonne Investigation of irradiation-induced Center for Advanced Energy Studies – National recrystallization in U-Mo fuel Microscopy and Characterization Suite Laboratory Ben Maier University of APT studies of irradiated cold spray Center for Advanced Energy Studies – Wisconsin coatings for accident tolerant cladding Microscopy and Characterization Suite Benjamin University of Site-specific APT characterisation of grain Center for Advanced Energy Studies – Jenkins Oxford boundaries in archival surveillance steels Microscopy and Characterization Suite from Advanced Test Reactor (ATR-2) neutron irradiation experiment Cem Topbasi Electric Power In situ TEM study of radiation damage Oak Ridge National Laboratory – Research effects on the δ-Hydride microstructure in Low Activation Materials Development Institute irradiated Zircaloy-4 and Analysis (LAMDA) Chi Xu University of An in situ TEM characterization of tensile Argonne National Laboratory Florida testing of ion irradiated HT-UPS steel at RT – Intermediate Voltage Electron and 400°C Microscope Tandem Facility David Massachusetts Post-irradiation analysis of hybrid metallic Oak Ridge National Laboratory – Low Carpenter Institute of coatings on SiC after neutron irradiation Activation Materials Development and Technology 290-330°C Analysis (LAMDA) Djamel North Carolina Ion irradiation response of nanostructured Argonne National Laboratory Kaoumi State University alloys: in situ TEM observations vs. ex situ – Intermediate Voltage Electron characterization Microscope Tandem Facility

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PI Name Institution Title Facility

Elena Tajuelo Oak Ridge Changes on viscoelastic behavior, Oak Ridge National Laboratory – Low Rodriguez National morphology and chemical structure Activation Materials Development and Laboratory of gamma irradiated calcium silicate Analysis (LAMDA) hydrates to 1.94 MGy with respect to non-irradiated samples Erik Mader Electric Power AsTeROID (follow-on AsTeR (Advanced Idaho National Laboratory – Materials Research Test Reactor) project to Optimize and Fuels Complex Institute hydrogen-assisted Irradiation growth and Dimensional stability) Gabriel Meric University of The effectiveness of coherent and Argonne National Laboratory de Bellefon Wisconsin incoherent twin boundaries in alleviating – Intermediate Voltage Electron radiation damage in heavy ion irradiated Microscope Tandem Facility 316L austenitic stainless steels Elizabeth United States Radiation tolerance of advanced University of Michigan – Michigan Ion Getto Naval Academy joining techniques for oxide dispersion Beam Laboratory strengthened steels under ion irradiation Haiming Idaho State Enhanced irradiation tolerance of high- University of Wisconsin – Tandem Wen University entropy alloys Accelerator Ion Beam and the Characterization Laboratory for Irradiated Materials Konstantina SCK•CEN Study of the factors affecting the radiation University of Michigan – Michigan Ion Lambrinou tolerance of MAX phases for innovative Beam Laboratory fuel cladding concepts Kumar University of Heavy ion irradiation and ex situ University of Wisconsin – Tandem Sridharan Wisconsin transmission electron microscopy study Accelerator Ion Beam and the of the effectiveness of twin boundaries in Characterization Laboratory for alleviating radiation damage in Irradiated Materials 316 austenitic stainless steels Lin Shao Texas A&M Post-irradiation observation following Center for Advanced Energy Studies – University high rate self-ion irradiation of previously Microscopy and Characterization Suite neutron irradiated 304 stainless steel Mukesh Idaho National Microstructure and microchemical Center for Advanced Energy Studies – Bachhav Laboratory characterization of neutron and proton Microscopy and Characterization Suite irradiated alloy D9 using APT and TEM

77 Nuclear Science User Facilities

PI Name Institution Title Facility

Mukesh Idaho National Effect of Phosphorous (P) on precipitation Center for Advanced Energy Studies – Bachhav Laboratory and segregation behavior in neutron Microscopy and Characterization Suite irradiated Reactor Pressure Vessel (RPV) steels in the Advanced Test Reactor (ATR- 2): An atom probe study. Nathan University of APT investigations of nm-scale precipitates Center for Advanced Energy Studies – Almirall California, in advanced RPV super clean steels in Microscopy and Characterization Suite Santa Barbara the UCSB Advanced Test Reactor (ATR-2) neutron irradiation experiment Niels SCK•CEN Hardness profiling of ion irradiated University of California, Berkeley Cautaerts 15-15Ti cladding steel using CSM nanoindentation Philip Oak Ridge In situ amorphization studies of forsterite, Argonne National Laboratory Edmondson National diopside and quartz under ion irradiation – Intermediate Voltage Electron Laboratory Microscope Tandem Facility Riley Parrish University of Microstructural characterization of 13% Idaho National Laboratory – Materials Florida burn-up MOX fuel and Fuels Complex Riley Parrish University of Microstructural characterization of 21% Idaho National Laboratory – Materials Florida burn-up MOX fuel and Fuels Complex

Rodney Stanford Radiation tolerance of Mn+1AXn phase Argonne National Laboratory Ewing University nuclear fuel cladding materials – Intermediate Voltage Electron Microscope Tandem Facility Sebastien Idaho National Characterization of grain boundary University of California, Berkeley Teysseyre Laboratory damage in highly irradiated specimens exposed to irradiation assisted stress corrosion cracking Sebastien Idaho National Characterization of the stability of the Center for Advanced Energy Studies – Teysseyre Laboratory microstructure of novel ODS alloys Microscopy and Characterization Suite Steven Zinkle University of Irradiation responses of ultrastrong nano Center for Advanced Energy Studies – Tennessee precipitation martensite steel Microscopy and Characterization Suite

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Fuel transfer at the Transient Reactor Test Facility, MFC, INL (Chris Morgan, INL) 79 Nuclear Science User Facilities

PI Name Institution Title Facility

Tianyi Chen Oak Ridge Radiation hardening and microstructural Center for Advanced Energy Studies – National stability of NF709 austenitic stainless steel Microscopy and Characterization Suite Laboratory Todd Allen University of Examining microstructural differences in Idaho National Laboratory – Materials Wisconsin irradiated HT9, correlated with differences and Fuels Complex in processing prior to irradiation Todd Allen University of IVEM investigation of defect evolution Argonne National Laboratory Wisconsin in FCC and BCC HEAs during heavy ion – Intermediate Voltage Electron irradiation Microscope Tandem Facility Weiying Argonne Fundamental study of alloying complexity Argonne National Laboratory Chen National effects on the irradiation process in high – Intermediate Voltage Electron Laboratory entropy alloys Microscope Tandem Facility Yong Yang University of Characterize the irradiated microstructure Center for Advanced Energy Studies – Florida and understand the fission product Microscopy and Characterization Suite behavior in an irradiated and safety tested AGR-1 TRISO fuel particle new proposal Yuanyuan Pacific Microstructural examination of neutron Pacific Northwest National Laboratory –

Zhu Northwest irradiated Al-HfAl3 metal matrix Radiochemistry Processing Laboratory National composite materials for application to Laboratory neutron spectrum modification in nuclear reactors Zheng Zhang University of Pore size distribution in U-Mo fuel Idaho National Laboratory – Materials Florida irradiated to low burnup and Fuels Complex

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FY 2017 Consolidated Innovative Nuclear Research (CINR) Awards In FY 2017, DOE selected five will support six of these projects neutron and ion irradiation testing, university, five national laboratory, with a total of $2.3 million in post-irradiation examination facili- and five industry-led projects that research funds, and all 15 of these ties, synchrotron beamline capa- will take advantage of NSUF capabil- projects will be supported by more bilities, and technical assistance for ities to investigate important nuclear than $10 million in facility access design and analysis of experiments fuel and material applications. DOE costs and expertise for experimental through the NSUF.

Joint R&D with NSUF Access

Title Institution Project Description

NSUF Project 17-12527: Boise State Researchers will develop and demonstrate an additive manufacturing Additive Manufacturing University approach to fabricate nonintrusive and spatially resolved sensors for of Thermal Sensors for in-pile thermal conductivity measurement. The team will print thermal in-pile Thermal Conductivity conductivity sensors onto fuel components using an aerosol jet printing Measurement approach, and study in-pile performance of the printed sensors through irradiation and post-irradiation testing. This research has the potential to establish a new sensor manufacturing paradigm for the nuclear industry. NSUF Project 17-12573: General Researchers will investigate the effects of temperature and thermal Performance of SiC-SiC Atomics gradients on the irradiation performance and stability of joints in silicon Cladding and Endplug Joints carbide (SiC) cladding and endplug geometries. The project will fill a under Neutron Irradiation gap in understanding the performance SiC joint performance which will with a Thermal Gradient advance the development of accident tolerant fuels. NSUF Project 17-13004: Los Alamos Researchers will join cladding tubes of 14YWT alloy and a ferritic ODS Capacitive Discharge National alloy using capacitor-discharge resistance welding (CDRW), a rapid, Resistance Welding of Laboratory solid-state welding process with very low heat input. The CDRW process 14YWT for Cladding is especially well suited for cladding applications. The project will Applications provide a significant advance in the state of the knowledge for joining of 14YWT and ferritic ODS materials and will permit their broader use with increased confidence.

81 Nuclear Science User Facilities

Title Institution Project Description

NSUF Project 17-13050: Oak Ridge Researchers will identify correlations between microstructures Correlation between National and mechanical properties of neutron irradiated advanced ferritic- Microstructure and Laboratory martensitic and austenitic steels through comprehensive experimental Mechanical Properties of post-irradiation examinations, coupled with thermodynamics, kinetics Neutron-Irradiated Ferritic- and microstructural hardening modeling of selected samples that are Martensitic and Austenitic relevant to Light Water Reactors. Results from other ongoing studies Steels and literature data of similar alloys will be collected and compared to complement the correlations. NSUF Project 17-12797: Pennsylvania Researchers will add the capability to model irradiation assisted grain

In Situ Ion Irradiation to State growth to the MARMOT tool by using in situ ion irradiation of UO2 Add Irradiation Assisted University to quantify the effect of irradiation on grain growth. The team will Grain Growth to the investigate the hypothesis that irradiation assisted grain growth is caused MARMOT Tool by thermal spikes resulting from atom collisions. The model added to MARMOT will couple the existing grain growth model to a heat conduction simulation using a stochastic heat source describing the thermal spike. NSUF Project 17-13073: University of Researchers will establish the foundation for converging disciplines Radiation Effects on Pittsburgh of multi-functional fiber optic sensors and additive manufacturing Optical Fiber Sensor Fused for smart part fabrications for nuclear energy applications, especially Smart Alloy Parts with for in-pile applications. Using advanced laser fabrication techniques, Graded Alloy Composition the team will develop both high-temperature stable point sensors and Manufactured by Additive distributed fiber sensors for high spatial resolution measurements in Manufacturing Processes radiation-hardened silica and sapphire fibers.

82 2017 | ANNUAL REPORT

NSUF Access Only

Title Institution Project Description

NSUF Project 17-13007: AREVA To provide irradiation and post-irradiation examination program for four Irradiation of Advanced neutron absorber materials. The team will evaluate four pellets of each Neutron Absorbing Material absorber type irradiated to target doses of 1.3 and 2.7 x 1022 n/cm2. to Support Accident Tolerant Following neutron irradiation, examinations will focus on pellet integrity Fuel using optical microscopy and dimensional measurements to characterize irradiation induced swelling. This scope of work will utilize HFIR and hot cells at ORNL. NSUF Project 17-12985: Electric Researchers will provide experimental data on fuel fragmentation’s role Irradiation, Transient Power in fuel burnup to make the case for increasing the regulatory burnup Testing and Post Irradiation Research limit past 62 Gwd/MTU. The scope of work involves re-irradiation of Examination of Ultra High Institute, Inc. high burnup fuel at the appropriate power levels in ATR followed by Burnup Fuel transient testing, both out of reactor and in TREAT. NSUF Project 17-12957: Oak Ridge The proposed work at the NSLS-II Facility will conduct synchrotron- X-ray Characterization of National based XRD experiments on high-purity SiC neutron irradiated with and Atomistic Defects Causing Laboratory without applied stress. The outcome from this work will provide critical Irradiation Creep of SiC experimental data to understand underlying mechanism of irradiation creep of SiC and will consequently advance the thermo-mechanical model of the SiC cladding of LWRs. NSUF Project 17-13088: Electric Researchers will study why Zircaloy-2 material shows high hydrogen Improved Understanding of Power pickup and variability in BWR environments by investigating the Zircaloy-2 Hydrogen Pickup Research correlation between the irradiated Zircaloy-2 oxide layer resistivity and Mechanism in BWRs Institute, Inc. hydrogen pickup. The scope of work will include in situ electrochemical impedance spectroscopy (EIS) measurements on pre-irradiated channel and water rod samples as well as post-irradiation characterization of the same materials using Transmission Electron Microscopy and Scanning Electron Microscopy at PNNL. NSUF Project 17-12976: Idaho Researchers will grow the available database of post irradiation data Study of the Irradiation National available for annular mixed oxide (MOX) fuel irradiated in fast spectrum Behavior of Fast Reactor Laboratory reactors by examining irradiated fuel from the FO-2 irradiation. The Mixed Oxide Annular Fuel data collected in this project would be used to validate models currently with Modern Microstructural being developed at the Japanese Atomic Energy Agency (JAEA) for fuel Characterization to Support performance models that seek to simulate MOX fuel behavior and will Science Based Model be implemented in BISON. Validation

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Title Institution Project Description NSUF Project 17-12849: Pacific Researchers will develop atomic scale data on the phase stability and Simulation of Radiation and Northwest thermo-mechanical properties of FeCrAl accident tolerant cladding Thermal Effects in Advanced National under the combined effects of radiation and elevated temperature. The Cladding Materials Laboratory goal is to ultimately provide materials parameters for the MARMOT code and develop predictive physics-based models for the BISON code. NSUF Project 17-13211: University Researchers will quantitatively measure sub-5nm defect structures, Positron Annihilation Studies of Illinois, particularly tiny vacancy clusters, which are inaccessible using any other of Neutron Irradiated Urbana- microstructural analysis techniques. The project will use North Carolina Ferritic Alloys Champaign State University’s PALS and DBS systems to study nanoscale defect structures in ATR neutron irradiated ferritic and ferritic/martenistic alloys. NSUF Project 17-12853: University of Researchers will develop high-performance simulation tools to predict HPC Access to Advance Tennessee, fission gas bubble evolution in nuclear fuel. The scope of work in this Understanding of Fission Knoxville project includes access to 10 million CPU hours of high performance Gas Behavior in Nuclear Fuel computing (HPC) resources each year for two years. NSUF Project 17-13106: Westing- Researchers will collect post irradiation examination data for additive Radiation Effects on house manufactured Zircalloy-2 materials for LWR fuel applications. The scope Zirconium Alloys Produced Electric of work includes PIE of a previously irradiated zirconium material that by Powder Bed Fusion Company was fabricated using laser powder bed fusion. The sample was irradiated Additive Manufacturing at MIT’s reactor and PIE will be conducted at Westinghouse’s Churchill Processes hot cell facility.

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A researcher working in the In situ Ion Irradiation Scanning Electron Microscope (I3SEM) Facility, Sandia Ion Beam Laboratory, Sandia National Laboratories (Courtesy of Sandia National Laboratories) 85 Nuclear Science User Facilities

NSUF ACROSS THE NATION

Paci c Northwest National Laboratory IDAHO NATIONAL LABORATORY Massachusetts Institute of Technology

Center for Advanced University of University Wisconsin, Madison of Michigan INL Energy Studies University of Brookhaven California, Berkeley The Ohio Westinghouse National Illinois Institute State Laboratory of Technology University Lawrence Livermore Purdue National Laboratory University Argonne National Laboratory University of Nevada, Las Vegas North Carolina Oak Ridge National State University Sandia National Los Alamos Laboratory Laboratories National Laboratory

Texas A&M University University of Florida PIs/User Institutions Partners (As of 2018)

NSUF Partner Institutions

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Participants at the first NSUF Partner Facilities Workshop, Center for Advanced Energy Studies (CAES) (May 2017) (Chris Morgan, INL)

NSUF User Institutions

Arizona Maryland Tennessee Arizona State University The Johns Hopkins University Oak Ridge National Laboratory United States Naval Academy University of Tennessee California Vanderbilt University Electric Power Research Institute (EPRI) Massachusetts General Atomics Massachusetts Institute of Technology Texas Stanford University Texas A&M University Michigan University of California, Berkeley University of Houston Michigan State University University of California, University of Michigan Utah Santa Barbara University of Utah Missouri Colorado Utah State University University of Missouri Colorado School of Mines Virginia New York Florida AREVA NP Rensselaer Polytechnic Institute (RPI) Florida State University Virginia Commonwealth University University of Central Florida Nevada Washington University of Florida University of Nevada – Las Vegas Pacific Northwest Idaho New Mexico National Laboratory Boise State University Los Alamos National Laboratory Wisconsin Idaho National Laboratory Sandia National Laboratories University of Wisconsin Idaho State University North Carolina University of Idaho GE Hitachi Nuclear Energy Australia Illinois North Carolina State University Australian Nuclear Science and Technology Organization Argonne National Laboratory Ohio Illinois Institute of Technology The Ohio State University Belgium University of Illinois University of Cincinnati SCK•CEN Indiana Oregon France Purdue University Oregon State University CEA Saclay Kansas Pennsylvania United Kingdom Kansas State University Drexel University Oxford University Pennsylvania State University University of Liverpool University of Pittsburgh University of Manchester Westinghouse

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The Control Room for the Advanced Test Reactor (ATR), INL (Chris Morgan, INL) 88 2017 | ANNUAL REPORT

NSUF AWARDED PROJECTS This section contains reports on projects awarded through the NSUF and completed in FY 2017.

INL Advanced Test Reactor Complex Named ANS Nuclear Historic Landmark May 2017

he American Nuclear Society Today, the ATR remains the largest (ANS) dedicated the Idaho test reactor in the world with a TNational Laboratory (INL) unique serpentine fuel arrange- Advanced Test Reactor Complex as ment. The available experimental an ANS Nuclear Historic Landmark space of the ATR is shared by the U.S. at a May 2017 award ceremony. The Department of Energy, commercial complex housed the original Materials users, other nations, Nuclear Science Testing Reactor (MTR) built in 1952, User Facilities users, and the U.S. Navy. the Engineering Test Reactor (ETR) in It is still revered as the nation’s premier 1957, and the Advanced Test Reactor resource for fuels and materials irradia- (ATR) that began operation in 1967. tion testing, nuclear safety research, and nuclear isotope production. At the INL Advanced Reactor Complex dedication, ANS President Andrew The INL Advanced Test Reactor was Klein said, “The INL Advanced Reactor recognized in 2016 with the ANS Complex has valuable history in Meritorious Performance in Opera- nuclear energy research, safety, and tions Award. The national award recog- security. The work performed at the nizes outstanding performance in the complex today will help us meet operation of nuclear facilities. The current nuclear challenges and develop Advanced Test Reactor is marking its future advanced reactor technologies.” 50-year anniversary in 2017.

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Nanohardness measurements on neutron irradiated steel samples for next generation reactors Tarik Saleh – Los Alamos National Laboratory – [email protected]

Figure 1. Plot comparing os Alamos National Laboratory Project Description predicted σni using H1000 values has samples from a large The mechanical testing data at from hc to σy and σflow for the ATR-irradiated samples. Note Lnumber of neutron irradiation different length scales (macroscopic to that σni,y = σni,flow for the Milot experiments in their hot cells. nano) at varying doses and irradiation correlation. Green line indicates Most of these samples have, or will temperatures in assorted materials will 1:1 agreement, while red/blue have, macroscopic mechanical test increase the understanding of funda- lines indicate +/− 10%. data (tensile or shear punch tests) mental irradiation effects in candidate performed on them. This proposal cladding materials for next generation covered sending undeformed reactors and current reactor accident sections of these irradiated samples tolerant claddings (Figure 1). The to UC Berkeley for nanoindentation data collected from this work can feed and imaging of samples. The directly into finite element method combination of the macroscopic (FEM)-based models of true stress- mechanical property measurements strain constitutive behavior of irradi- and the nanoindentation data fed into ated materials, including strain rate constitutive modeling of irradiated and multiscale behavior. This ability materials, resulting in a mechanistic to extrapolate macroscopic mechanical understanding of irradiation effects property data from small samples on the mechanical behavior of next via small scale testing and modeling generation and accident tolerant will allow for more efficient use of cladding materials. neutron irradiation experiments, leading to advances in understanding high dose materials behavior.

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Access to LANL expertise and irradiated samples through the NSUF has been pivotal in the development of radioactive material handling and testing capabilities at UC Berkeley. In Figure 2. Photograph of polishing setup in radioactive material fume hood in 1140 Etcheverry Hall, UC Berkeley. An overview of the space including a MiniMet semiautomatic polisher, lead walls, and surface sheets for shielding. addition, the data generated from

Accomplishments processing methods to accurately Initial work, beginning in 2016, compare data between traditional and this collaboration has played included shipping samples from Los instrumented indentation methods that Alamos National Laboratory Wing 9 depends on expected sample strain- a key role in advancing not hot cells to UC Berkeley and continued hardening characteristics. As many development of a robust shielded of the empirical correlations linking sample holder for polishing the irradi- hardness to bulk tensile properties use only my thesis work but other ated samples in hoods, and handling optically measured Vickers microhard- and transfer between instruments ness, understanding the link between collaborative projects within (Figures 2 and 3). Work on character- that measure of hardness and the izing the Advanced Test Reactor (ATR) results from nanoindentation is vital. irradiated samples continued in 2017. DOE NEUP. After determining best practices Both micro and nano scale Berkovich to process the nanoindentation indentation was performed on all data, hardness results were directly eight samples in both irradiated and — David Krumwiede, Student compared to LANL-measured tensile as-received conditions. This data was properties utilizing three different cross-compared and also compared to empirical relationships. The efficacy previous Vickers microhardness data of each correlation was analyzed on to determine effects of test size and an alloy-by-alloy and overall basis indenter tip geometry. This analysis led to determining nonstandard data

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Figure 3. (Left) Photograph and (right) for a multitude of indentation curve in a shear punch system. The shear cross-sectional schematic of updated processing techniques. Details of these properties from these tests can be three-piece sample holder design for polishing small irradiated samples in analyses have been published in journal correlated with tensile properties. As hoods, shielded storage, and secure articles (publications [1,2]) and a Ph.D. such, nanohardness can be correlated transferring of samples between dissertation. In summary, with a proper with standard penetration test data via hoods and instruments. prediction of a sample’s strain-hard- a two-step process. This work validates ening behavior, both the yield stress one of those steps. Second, analysis and 8% flow stress can be estimated to of ion irradiated samples requires the within 5% of the measured property. use of small scale mechanical testing, Figure 1 shows correlation of measured such as nanoindentation. The ability NSUF Fuels & tensile and flow stress on macroscopic to extrapolate to bulk properties is an Materials Library irradiated samples compared to essential screening tool for an alloy’s 08-139 UCSB samples predicted data derived from nanohard- irradiation performance. ness data that was measured on the Future Activities same samples. For a full discussion, This research will expand beyond see publications [2]. the initial irradiation conditions The ability to use nanoindentation to in the Spallation Target Irradiation predict tensile properties is important Program (STIP) and ATR irradiations for future works for two reasons. First, to encompass samples from different future experiments will investigate irradiation conditions in the ATR samples from BOR60 that were irradi- and much higher dose irradiations ated as TEM discs, which were tested including BOR60 irradiations as well as archived samples from the Fast

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Formalizing relations between nanoscale and macroscopic mechanical data via experiment modeling will allow for more efficient testing and better understanding of high dose cladding material for next generation reactors.

Flux Test Facility. This will generate Congress on Advances in Nuclear a bigger database of macro and nano Power Plants, ICAPP 2016 Volume mechanical properties for model and 1, 2016, Pages 224-229 technique validation. [2.] D.L. Krumwiede, T. Yamamoto, T. Publications Saleh, S.A. Maloy, G.R. Odette, and [1.] Krumwiede, David L; Abad, M.D.; P. Hosemann, “Direct comparison Saleh, Tarik A.; Maloy, Stuart of nanoindentation and tensile Andrew; Odette, G. Robert ; et al. test results on reactor-irradiated “Initial Studies on the Correlation materials,” Journal of Nuclear of Nanohardness to Engineering- Materials. Volume 504, June 2018, Scale Properties of Neutron- Pages 135-143 Irradiated Steels.” International

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Los Alamos Chemical and Metallurgical Research Facility National Laboratory (Wing 9) University of California, Nuclear Materials Laboratory Berkeley Collaborators Los Alamos Dr. Tarik A. Saleh (principal investigator), National Laboratory Dr. Stuart A. Maloy (co principal investigator) University of California, Dr. Peter Hosemann (collaborator), Berkeley David Krumwiede (collaborator)

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Critical evaluation of radiation induced segregation in nickel base alloys subjected to proton irradiation Miao Song – University of Michigan – [email protected]

adiation induced segregation structural integrity in harsh radiation (RIS) behavior is used as environments. Over the past years, Rone of the indicators of the the Electric Power Research Institute radiation resistance of materials for (EPRI) tried to identify all possible its potential impacts on irradiation degradation mechanisms and their assisted stress corrosion cracking potential effects on the reactor (IASCC).The RIS behavior of several components. Void swelling, stress The data related to commercial austenitic alloys (alloy corrosion cracking (SCC), IASCC, radiation induced 625, 625Plus, 625DA, 725, 800 and and fracture toughness are the major segregation can impact 310) was investigated. All the alloys concerns as materials experience the material selection were proton irradiated to 5 dpa at high irradiation levels. However, for the life extension of 360°C in the Michigan Ion Beam most in-core structures were built current operating light Laboratory (MIBL). Energy-dispersive with austenitic stainless steels, which water reactors with X-ray spectroscopy (EDX) scans are susceptible to degradation at a better safety were performed on a Talos scanning relative early time during service. and efficiency. transmission electron microscope Thus, replacement components may (STEM) in the Low Activation become a necessity. EPRI initiated Materials Design and Analysis the Advanced Radiation Resistant Laboratory at ORNL. RIS results Materials (ARRM) program to address show that all the random high-angle these issues. The ARRM project is grain boundaries of these austenitic aimed at identifying promising alloys follow the same pattern of candidate alloys that can replace significant Cr and Fe depletion and Ni austenitic stainless steels, which enrichment. RIS of minor elements suffer from serious IASCC in light such as Si in austenitic steels were water reactor (LWR) environments. tracked as well. These results can Reactors using these alloys can provide the knowledge to identify operate with better efficiency and the most promising radiation tolerant lower cost of maintenance and repair. alloys with good resistance to IASCC. The successful completion of this proposed project will facilitate the Project Description completion of the ARRM project, The life extension of current which aligns well with the first existing reactors and design of next program goal: development of new generation nuclear reactors require nuclear generation technologies advanced materials that can maintain and proliferation-resistant LWR and fuel cycle technologies, and development and deployment of next

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Figure 1. EDX mapping of irradiated alloy 725: (a) bright field image of a triple junction, (b) the target grain boundary and mapping area. EDX mapping results of individual elements (c) Ni (d) Cr (e) Mo (f) Fe (g) Ti (h) Al and (i) Nb.

generation advanced reactors and fuel Accomplishments cycles in the longer term. Also, the IASCC is identified as one of the second phase of the ARRM project is primary degradation mechanisms targeting the development of superior for materials of core components in degradation resistant alloys, which LWR systems. Among all the factors, would allow a larger margin of design RIS, especially Cr depletion at grain and even tolerance for beyond- boundaries (GBs), is suspected to be design-basis events. This addresses a contributor to the susceptibility of the second program goal: enhancing IASCC. Ni base alloys and austenitic the safety of the nation’s nuclear stainless steels typically exhibit infrastructure to meet national energy and environmental needs.

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Figure 2. Comparison of (a) irradiation induced segregation and (b) GB chemistry in several Ni based alloys.

excellent mechanical properties The first issue is to determine random and good resistance to corrosion. high-angle grain boundaries. The triple However, the data related to RIS are junctions are applied to distinguish limited to alloys 316 and 304. The the random high-angle GB from a goal of this study is to evaluate the twin boundary. The Kikuchi patterns RIS behavior of nickel- and iron- for both grains are also recorded for based austenitic alloys 625, 625Plus, precise misorientation calculation. After 625DA, 725, 800 and 310, which are the targeted GB type is determined, the rarely reported in literature. grain boundary is tilted to an edge-on condition for EDX analysis. The EDX Random high-angle GBs are typically mappings are performed across the susceptible to IASCC. These GBs possess GBs. The 2D mapping data are trans- a length fraction of ~30% in alloy 625, ferred into 1D lines, corresponding in ~22% in alloy 625Plus, ~46% in alloy area to the width of the box (>100nm) 718, ~32% in alloy 725, ~49.3% in across the GBs in Figure 1. Good signal alloy 310, and ~32.4% in alloy 800, to noise ratio was achieved. based on the electron backscatter diffraction (EBSD) study.

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Figure 3. Grain boundary segregation before and after irradiation in several commercial grade alloys: (a) as-received (AR) alloy 725 and (b) irradiated alloy 725, (c) AR alloy 800 and (d) irradiated alloy 800, (e) AR alloy 310, and (f) irradiated alloy 310.

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Based on this method, grain boundary Segregation in as-received stainless segregation was observed in all alloys steels is insignificant, as shown in investigated. In Ni based alloys, deple- Figure 3 where only a small amount tion of Ni and enrichment of Cr and of segregation was observed. However, Mo were observed in the as-received the RIS is significant. The general alloys. The segregation seems smaller pattern is the same as in the Ni based in alloy 625DA, likely due to a lower alloys in which significant Ni diffuses aging temperature. After irradiation, to the GB and Cr and Fe diffuse significant Ni enhancement was away from the GB. The RIS of Si is observed in the Ni based alloy while pronounced, typically about three Cr and Fe were always depleted. Mo times its nominal value. In alloy 800, was a slow diffuser that is enriched in the amount of Si at the GB is compa- the as-received materials and depleted rable to that of Cr while the nominal under irradiation. The segregation of composition of Cr is more than 40 other elements is either insignificant times that of Si in the alloy. or beyond the resolution of equip- Alloy 800, with 31Ni-22Cr-45Fe, ment. A comparison of RIS in the shows the highest magnitude of Ni based alloys is summarized in radiation induced segregation. Both Figure 2. 625DA shows the lowest Ni based and Fe based alloys show GB Cr level of around 8 wt%. The less segregation compared to alloy Ni concentration increases up to 70 800. The segregation behaviors of wt%, which is around 10 wt% above the elements are consistent among the bulk composition. The difference different alloys: Ni is always enriched between different Ni based alloys is after irradiation, and Cr and Fe insignificant. The RIS in stainless steels are depleted. These data constitute are presented separately due to their important knowledge of the RIS in different chemical composition. commercial grade alloys. Dr. Chad M. Parish at Oak Ridge National Laboratory is acknowledged for the successful completion of the project.

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Publications [2.] W. Kuang, M. Song, C. Parish, G. [1.] M. Song, M. Wang, G. Was, L. Was, Microstructural Study on the Nelson, R. Pathania, Irradiation Stress Corrosion Cracking of Alloy Assisted Stress Corrosion Crack- 690 in Simulated Pressurized Water ing (IASCC) of Nickel-base Alloys Reactor Primary Environment, 18th in Light Water Reactors Environ- International Conference on Envi- ments Part I: Microstructure ronmental Degradation of Materi- Characterization, 18th Interna- als in Nuclear Power Systems – Wa- tional Conference on Environ- ter Reactors, August 13-17, 2017, mental Degradation of Materials Portland, Oregon, USA in Nuclear Power Systems – Water Reactors, August 13-17, 2017, Portland, Oregon, USA

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Oak Ridge Low Activation Materials Design National Laboratory and Analysis Laboratory Collaborators Electric Power Raj Pathania (co principal investigator) Research Institute Oak Ridge Keith Leonard (co principal investigator) National Laboratory University of Michigan Gary Was (co principal investigator), Miao Song (principal investigator), Mi Wang (co principal investigator)

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A comparison of mechanical properties of ion and neutron irradiated Fe-9Cr Professor Steve Roberts – University of Oxford – [email protected]

Figure 1. A FIB-milled microcantilever in neutron irradiated Fe-9Cr alloy. These cantilevers are deformed, using a nanoindenter as a loading device, to give yield and flow data from very small volumes of material.

Ion irradiation can be a cheaper and faster surrogate for neutron irradiation in the study of radiation damage effects, but whether it is a valid surrogate or not can depend strongly on small changes in alloy composition. These experiments have eutron irradiation campaigns Heavy ion irradiation provides a helped us understand are expensive, take a faster, cheaper alternative to neutron this better. Nsignificant amount of time irradiation where good control over to complete, and offer only limited experimental parameters allows a control over experimental conditions. methodical approach towards building Radioactivity is also induced in an understanding of radiation damage, samples, requiring specialized without the need for irradiated mate- handling facilities, such as provided rial handling facilities. by the NSUF, that are not routinely This work uses small scale mechanical available to most researchers. testing and microstructural analysis techniques to study how well heavy ion irradiation replicates neutron irradiation in a nuclear relevant model alloy.

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Project Description Understanding the microstructural Figure 2. (a) Hardness and (b) The aim of this project is to compare development of these alloys under fractional increase in hardness after ion and neutron irradiation the mechanical properties and micro- irradiation is critical for the design, for FeCr model alloys. Points of structure of samples of an Fe-9Cr safe operation, and commercial the same composition have been model alloy irradiated under the same viability of future reactors. spread horizontally slightly for conditions using heavy ions at the ease of reading. Nanoindentation Heavy ion irradiation has often been hardness data were taken at Joint Accelerators for Nanosciences used to study radiation damage 300 nm indenter penetration and NUclear Simulation (JANNuS) in these materials. The damage using the cross-section method. facility in Saclay-Orsay, France, and Fe6Cr nanoindentation data from produced by this technique has with neutrons in the Advanced Test C.Hardie (University of Oxford/ several neutron atypical character- CCFE), Fe-9Cr nanoindentation Reactor (ATR) at INL. istics, so it is important to validate data from L.Hewitt (University of Oxford). Vickers hardness data Low activation ferritic/martensitic these experiments through compari- (500 g) provided by T. Milot (INL). steels with 9–12% Cr are favored sons with neutron irradiation made candidate materials for use in future possible through access to facilities fission and fusion reactors due to both provided by the NSUF. their superior swelling resistance at The shallow damage layer produced high doses compared to austenitic by heavy ion irradiation necessitates steels and an observed minimum in the use of small scale mechanical ductile to brittle transition temperature increase at this composition.

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Figure 3. Yield stress measured using simple beam theory on Fe-9Cr microcantilevers as a function of beam height for ion irradiated, neutron irradiated, and as-received samples. Each point represents a different microcantilever beam. Data produced by L. Hewitt (University of Oxford).

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testing methods such as nanoindenta- over a much shorter time, the dose tion and micromechanical testing. The rate differs significantly between the development of these techniques is two irradiation conditions. also of use for active materials—here, The FIB work on this and a reference reducing the size of samples required as-received sample was performed at reduces their activity, facilitating easier the University of Oxford, with testing Irradiation effects are handling and testing. and nanoindentation for all samples Accomplishments performed at CCFE. complicated – and the more The neutron irradiated sample had Changes in nanoindentation hard- already been irradiated to 1.7dpa at ness are shown in Figure 2, alongside 288°C as part of the University of experiments we do, the more similar work on an Fe-6Cr alloy from California at Santa Barbara (UCSB) this specimen series, performed as NSUF Irradiation Experiment lead by part of another NSUF project by C. complicated we find they are. G.R. Odette. The sample was provided Hardie of University of Oxford/ and prepared by P. Wells and D. Gragg CCFE. Data provided by T. Milot of INL at UCSB and shipped to the Center But we now have the tools to showing changes in Vickers hardness for Advanced Energy Studies (CAES). after neutron irradiation for both Microcantilever specimens alloys are also shown. understand what’s happening. (Figure 1) were then manufactured using the NSUF-funded access to Both the nanoindentation and Vickers the focused ion beam (FIB) at the hardness data show, for neutron — Steve Roberts, Professor of Microscopy and Characterization irradiation, a larger increase in Suite (MaCS) before being shipped hardness (absolute or relative) for the Materials, Oxford University, UK to the Materials Research Facility at Fe-6Cr alloy compared to the Fe-9Cr the Culham Centre for Fusion Energy alloy. The nanoindentation data show (CCFE), Culham, U.K., for testing. a greater disparity in the increase in Access to the MaCS facility was essen- hardness for ion and neutron irradia- tial to the feasibility of the research, as tion in the Fe-6Cr alloy than in the such active-material facilities were not Fe-9Cr alloy. This is thought to owe otherwise available to L. Hewitt. to dose-rate sensitivity of radiation induced changes in hardness, which The ion irradiated sample was irradi- has been shown to vary strongly ated at the JANNuS facility at the same with Cr content (Journal of Nuclear temperature, but due to technical Materials 439 [2013] 33–40). issues received a dose around 0.4–0.8 times that targeted. Because the ion irradiation was performed

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The yield stress measured by the irradiation induced hardening microcantilever testing shown in is not sensitive to possible radiation Figure 3 for the Fe-9Cr alloy also induced clustering of Cr, but depends displays similar changes after ion and more strongly on the presence of neutron irradiation. Data are more other radiation induced features such scattered than for the indentation as dislocation loops, which are less studies (this is thought to be due to sensitive to irradiation rate. small variations in beam dimensions, Note that the earlier work by Hardie to which the results are very sensitive: (also carried out with NSUF support) further analysis is in progress). Both indicates that the sensitivity of irra- ion irradiated beams and neutron irradiation hardening to dose rate (and diated beams show higher yield stress hence irradiation type, ion or neutron) values than unirradiated material. varies strongly with Cr content; for Analysis of the ion irradiated Fe-9Cr his Fe-6Cr, the slower irradiation with sample by atom probe tomography at neutrons gave a greater degree of hard- the University of Oxford revealed an ening than that for the rapid irradiation absence of the alpha prime precipi- with ions, which was not the case for tates in neutron irradiated Fe-9Cr the Fe-9Cr studied here. This may be materials found by M. Bachhav of due to a segregation of Cr to disloca- the University of Michigan (Scripta tion loops in Fe-6Cr. Further investiga- Materialia 74 (2014) 48–51); this tion is needed as these dose rate/%Cr/ likely owes to the large differences temperature (probably) effects have in irradiation rate between the ion a strong and controlling effect on the (fast ~3–6 × 10-5 dpa/s) and neutron extent to which hardening effects of (slow ~3 × 10-7 dpa/s) irradiation. neutron irradiation in this material type Because changes in hardness and can be evaluated by ion irradiation. properties under neutron irradiation were well reproduced by ion irradiation for this Cr content, it appears that

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This work highlights the need to vali- Further Vickers hardness tests will NSUF Fuels & date heavy ion irradiation experiments be performed with lower loads to Materials Library with work on neutron irradiated investigate size effects and samples, only possible through access provide continuity with the 08-139 UCSB samples to facilities such as those in MaCS at nanoindentation tests. CAES. It also shows the need for more Further microstructural analysis work to improve understanding of of the samples will be carried out, Cr behavior under irradiation for the particularly of dislocation loop design of ferritic/martensitic steels for chemistry, in order to understand future nuclear applications. and link the differences in Future Activities mechanical properties observed This work will be written up for for the different compositions to journal publication in 2018. damage microstructure.

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Idaho National Laboratory Advanced Test Reactor Collaborators University of Idaho Joanna Taylor (collaborator) University of California David Gragg (collaborator), Santa Barbara G.R. Odette (collaborator), Peter Wells (collaborator) University of Oxford Luke Hewitt (collaborator), Professor Steve Roberts (principal investigator)

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Influence of neutron irradiation on the microstructures and electrical properties of polymer derived ceramic sensing material Dr. Cheryl Xu – Florida State University – [email protected]

Figure 1. XRD pattern of 1600°C sintered SiC samples before and after irradiation.

If our hypothesis—that the microstructures and electrical properties are maintained under irradiation—is correct, these materials will later be used to create temperature sensors ensors fabricated of polymer- behavior, and piezoresistive behavior in a nuclear reactor for derived ceramics (PDCs) are up to temperatures higher than in-core temperature widely investigated. This kind of 1600°C. In the development of a measurement during the S material has shown a great potential sensor for use in high temperature next phase of research. for applications in high temperature and harsh environments, PDCs are and harsh environments that are one of only a few choices available. not survivable for most commercial In nuclear reactors, irradiation energy sensors available. Unlike conven- and temperature cause most materials tional polycrystalline ceramics, PDCs to degrade with time. For PDCs to possess a unique structure that can be be useful as a temperature sensor generally described as an amorphous inside a reactor, their irradiation matrix containing self-assembled resistance is very important. In this carbon phase (named free carbon project, investigation into irradiation in later discussion). Such a structure influence on the microstructure and leads to many unusual properties, electrical properties of PDCs will such as high temperature stability, proceed to determine the irradiation creep resistance, semiconducting resistance of PDCs.

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Figure 2. XRD pattern of 1600°C sintered SiOC samples before and after irradiation.

Project Description is the continuous generation of The objective of this project is to vacancies and interstitials in atomic perform neutron irradiation damage displacement cascades and defect tests on silicon-based PDCs. If our accumulation. Crystallinity of the hypothesis—that microstructure and material is thus an important factor electrical properties are maintained in radiation damage. PDCs are mostly under irradiation—is correct, such used at non crystalline state, which material will later be designed as makes them damage resistant. PDCs a temperature sensor in a nuclear also exhibit a more stable structure reactor for in-core temperature than crystalline SiC and Si3N4, which measurement. This will be the goal for is inferred from their higher creep the next phase of research. Irradiation resistance and higher thermal stability. stability is one of the most important It was further demonstrated that factors in ensuring the performance PDCs are thermodynamically stable as of PDC sensor material for nuclear compared to the crystalline mixtures applications. It is well known that (SiC + Si3N4 + graphite) of the same the root cause of radiation damage

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Figure 3. XRD pattern of 1600°C sintered SiCN samples before and after irradiation.

compositions. Unlike conventional Accomplishments materials, the PDCs consist of In the experiment, we first cured the nanodomains created by intertwined liquid ceramic precursor and then graphene (aromatic carbon) sheets crushed it into powders using ball about 1–5 nm in size. The unique milling. To get different compositions, structure of PDCs can effectively especially those not commercially promote defect recombination to available such SiBCN and SiAlCN, we mitigate radiation damage. The did chemical modifications on the variations of these structures under ceramic precursor, including polysi- irradiation damage would be critical lazane. After crushing, we prepared for the development of the sensor in the amorphous samples in our own harsh environments. laboratory by pressing each powder into bullets and then doing pyrolysis

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Figure 4. XRD pattern of 1800°C sintered SiBCN samples before and after irradiation.

under one atmosphere pressure in For amorphous samples, no pressure nitrogen. In order to get dense and is applied, and the dwelling tempera- crystallized PDC samples, our collabo- ture is 1000°C during pyrolysis. For rator at the National Aeronautics and crystallized samples, the pyrolysis Space Administration (NASA), Glenn, temperature is 1600°C (SiC, SiCN, helped us to prepare the samples using SiOC) or 1800°C (SiAlCN, SiBCN) higher temperatures (over 1400°C) in and the sintering pressure is 8 ksi. a hot press. Our collaborator at North Note that only ceramic or pyrolyzed Carolina State University coordinated powders can be used as a feedstock and finished the radiation tests. We did for hot press treatment. For every our characterization in High Perfor- sample irradiated, an extra, unirradi- mance Materials Institute and Chemistry ated sample from the same batch is department at Florida State University. archived for comparison.

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Figure 5. XRD pattern of 1800°C sintered SiAlCN samples before and after irradiation.

Visually, the irradiated and unirradi- 2. For SiCN (Fig. 3) and SiBCN ated samples are almost the same. For (Fig. 4) samples, irradiation crystallized samples (samples treated increased the crystallinity. The at higher temperature in a hot-press), (002) peak of graphite is the according to the x-ray diffraction only major peak in XRD, which (XRD) results: means that crystallization of Si-B- C-N composites is not complete. 1. SiC and SiOC samples show little After irradiation for 10 hours, change on the crystallinity struc- the graphite peak for both SiCN ture after 10 hours of irradiation and SiBCN samples has a higher (Fig. 1). SiC maintained its crys- intensity, which means that the tallinity over 10 hours of irradia- input irradiation energy in- tion. SiOC is not crystallized even creased crystallinity. after 1600°C sintering (Fig. 2). Its amorphous structures are similar before and after irradiation.

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3. For SiAlCN samples, irradiation atomic-scale defects such as intersti- destroys the crystal structure tials, displacement, stacking faults, gradually (Fig. 5). The main and Frenkel defects. These defects are crystallized peak is also the (002) difficult to detect by SEM because the peak of graphite. With increas- scale is small, and defects do not lie ing the peak irradiation time, on the surface. intensity decreases continuously, Future Activities and the crystallized peak disap- We will do furthur inspection on the peared after 50 hours irradiation, samples in order to determine what which means that neutrons have happened during irradiation. First, we destroyed the crystal structure of will measure electrical conductivity the sample. changes before and after irradiation. In summary, SiC (crystalized) and Then, high temperature dielectrical SiOC (amorphorous) show better irra- properties will be tested using our diation resistance than other compo- high temperature dielectric properties sitions. Irradiation increased the measurement system (funded by DOD crystallinity of SiCN and SiBCN while, DURIP, Award No. W911NF-16-1- for SiAlCN samples, the irradiation 0516). Third, ultrasonic scanning will energy destroys the crystal structure be performed in order to confirm after 50 hours of irradiation. the large-scale defect distribution throughout the sample. X-ray fluo- Scanning electronic microscopy (SEM) rescence (XRF) characterization will was used to inspect the microstructure be used to confirm the composition of the samples. No obvious extra change (i.e., change in element defects were detected for any sample ratios) for the samples before and under SEM measurement. In principle, after irradiation. neutron irradiation will generate

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities North Carolina PULSTAR Reactor Facility State University Collaborators Florida State University Dr. Cheryl Xu (principal investigator)

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Beamline examination of a Hf-Al metal-matrix composite material Donna Post Guillen – Idaho National Laboratory – [email protected]

Figure 1. Irradiated specimen he capability for conducting to be useful as a shroud for a variety of mounted in a triple contained fast neutron irradiation tests in fuel and material experiments. sample holder sealed with a domestic facility is needed to Kapton tape for EXAFS T The overall objective of this research meet fuels and materials testing require- measurements. is to determine the effects of ments for advanced reactor programs. radiation damage on the material DOE has examined options to augment microstructure, and in turn how the existing nuclear facilities to enable resultant microstructure affects the fast neutron testing, which could be thermal and mechanical properties of brought on line in a few years, much the material, which ultimately affect sooner than–and at a fraction of the cost performance and function of reactor of–building a new fast flux test reactor. components fabricated from this A fast flux test capability can be achieved material. Additionally, there is interest by incorporating a special testing rig in the HfAl as an elevated tempera- into one of the ATR corner lobes. A 3 ture alloy for the semiconductor new material, comprised of hafnium industry and other applications. aluminide (HfAl3) particles in an aluminum matrix has been developed The end result, in terms of the data to achieve the required neutronic and and fundamental understanding thermal characteristics of such a system. obtained, directly supports DOE’s This metal matrix composite material is mission of providing clean, reliable very promising for use in the Advanced energy technologies and benefits the Test Reactor as a conduction cooled science community in general. neutron absorber and has the potential

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Accomplishments the HfAl3 100 vol % alloy was 69.7 wt% Synchrotron extended X-ray absorption Hf, 29.4 wt% Al, with 8300 to 9400 fine structure (EXAFS) spectroscopy ppm of Zr and trace amounts of other measurements were performed to elements, and the chemical composition

study the structural changes in local of the HfAl3 28.4 vol % alloy was 67.04 atomic environments, defect forma- wt % Al, 32.96 wt % Hf, with 8300 to tion, and the evolution of Hf-Al phases 9400 ppm of Zr and trace amounts of

caused by irradiation and annealing other elements. The HfAl3 intermetallic in HfAl3-Al metal matrix composites. was produced by casting Hf and Al in The discovery of new The experiments were performed at a centrifugal caster. The HfAl3 castings the Advanced Photon Source (APS) were crushed into powder that was Materials Research Collaborative Access mixed with (for the 28.4 vol% material) materials opens up new Team (MRCAT) beamline 10-ID-B, or without (for the 100 vol% material) which is equipped with a Si(111) aluminum powder and uniaxially hot realms of possibilities and monochromator consisting of a pressed to form pucks from which cryo-cooled first crystal and a 250 mm specimens were fabricated by electrical long second crystal, providing an discharge machining. makes possible what was not energy range of 4.8–30 keV with the The specimens examined here were first harmonic. The absorption spectra 5 mm dia. x 2.5 mm thick, 5 mm dia. before possible. were recorded at room temperature at x 0.8 mm thick, or 3 mm dia. x the Hf L3-edge (E =9.561 keV) and o 0.3 mm thick disks. Samples were the Zr K-edge (E =17.998 keV) in o irradiated for 1, 2, 3 or 4 cycles — Donna Post Guillen, fluorescence geometry for the solid (800.6, 1965.5, 3184.0 or 3984.6 Distinguished Research Engineer samples and transmission geometry MWd) in the Advanced Test Reactor for the powders. Reference materials at INL. The materials were annealed consisted of Hf and Zr foils and after irradiation when differential powders of HfO , HfAl , and H Al . 2 3 2 5 scanning calorimetry was performed. From the Al-Hf phase diagram, various The irradiated samples are from the additional intermetallic phases can NSUF Fuels and Materials Library (USU form, including Al Hf, Al Hf, Al Hf , 3 2 3 2 KGT-1407, 1389, 1533, 1401, 1456, AlHf, Al Hf , Al Hf , and AlHf . The 3 4 2 3 2 1496). Each sample was taped into a objective of this research is to deter- Kel-F insert inside of a beamline holder mine which phases are initially present with Kapton tape, forming a triple layer in the material and which phases form of confinement (seen in Figure 1). as a function of neutron irradiation and The triple-contained specimens were subsequent annealing. The key question then shipped from the INL Materials to be answered by this study is, “Do and Fuels Complex to the APS for the new phases form as a result of irradia- synchrotron radiation experiments. tion or annealing?” The EXAFS measurements were The materials examined were comprised conducted at room temperature on of either 100 vol % HfAl or 28.4 vol % 3 three different states of the material: (1) HfAl -Al. The chemical composition of 3 unirradiated, (2) irradiated-unannealed,

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Figure 2. Fourier transform of the k2-weighted spectrum as a function of bond distance for the 100 vol% HfAl3 material at the Hf edge for three different material states.

and (3) irradiated-annealed specimens three different material states exhibit a exposed to 0.40, 0.93, 1.05, 2.57, 3.51, decrease in the amplitude of (R) from Successful completion X and 3.65 displacements per atom (dpa) higher order shells (R > 3A˚). As the of this project will at 95-150 °C. The EXAFS data for the Hf signal is a superposition of the photo- provide necessary data L3-edge and Zr K-edge were recorded, electron scattering functions for each for the development and the local structure close to the X-ray shell, this suggests that in the annealed of a fast neutron test absorbing atom was determined. X-ray sample, the nearest neighbors around capability in existing absorption data for all samples were the Hf or Zr atoms are well defined, but light water reactors, fill processed and analyzed using Athena the outer atomic shell structure is more a knowledge gap on and Artemis software. The X-ray absorp- disordered. These results demonstrate the basic properties of tion spectrum for each sample is an that EXAFS can provide an atomic level the HfAl intermetallic 3 average of 10-15 scans that were initially description of radiation damage in metal and HfAl3-Al neutron processed using standard pre-edge back- matrix composite systems. absorbers, and ground subtraction, edge-step normal- advance the scientific The PIs are grateful to Professor Jeff ization, and energy calibration proce- understanding of the Terry for his expert knowledge in dures. The first large peak in the Fourier irradiation effects on conducting beamline experiments with transform of the k2-weighted spectrum, these materials. irradiated materials at MRCAT and to (R), as a function of bond distance, R, X Ph.D. student Rachel Siebert for her seen in Figures 2 and 3 is indicative of invaluable guidance on analyzing the the signal from the first shell of atoms. A EXAFS data. significant reduction in peak amplitude occurs in the Hf L3-edge and Zr K-edge Future Activities spectra for the irradiated-unannealed We will continue to analyze the data specimens. The irradiated-annealed obtained at the MRCAT beamline in specimens display an increase, but not a March 2017. Pair distribution func- full restoration, of the peak amplitude. tion data from synchrotron diffraction Irradiation damage is manifested by the experiments was obtained at the creation of local disorder within the Advanced Photon Source beamline crystal structure of the material, which 6-ID in July 2017. This complementary is partially restored by annealing. The data will be helpful to identify the phases present and the associated bond

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Figure 3. Fourier transform of the k2-weighted spectrum as a function of bond distance for the 100 vol% HfAL3 irradiated material and Hf2Al5 reference at the Zr edge.

distances. EXAFS data will be analyzed to the Al matrix) to radiation damage levels NSUF Fuels & quantitatively determine average bond of 1 and 3 dpa. This will provide needed Materials Library distance (r (Å)), coordination number information on the high temperature (n (atoms)), and disorder (Debye- stability of these materials in an irradia- 09-157 U of Utah Waller factor or σ2 (Å2)) of shells of tion environment. atoms around the absorbing atom. A Publications journal publication will be prepared [1.] Cheng, S. and Guillen, D.P., Charac- with these results. terizing Local Structure of Nuclear Additional future work planned to Materials Using X-Ray Diffrac- commence in spring 2018 includes tion and Spectroscopy Techniques, another ATR irradiation experiment presented at the INL Intern Expo, of the HfAl3-Al materials at sustained August 2017. *See additional temperatures of 300°C±50°C and publications from other years in the

400°C±50°C (~0.45Tm and 0.61Tm of Media Library on the NSUF website at nsuf.inl.gov.

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Illinois Institute Materials Research Collaborative Access of Technology Team (MRCAT) facility at Argonne National Laboratory’s Advanced Photon Source (APS) Collaborators Idaho National Laboratory Donna Post Guillen (principal investigator), Douglas Porter (principal investigator) Rutgers University Steven Cheng (intern)

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Atom Probe Tomography characterization of irradiated

UO2 fuel from the BR3 Belgium Reactor Brandon Miller – Idaho National Laboratory – [email protected]

Figure 1. Irradiated specimen mounted in a triple-contained sample holder sealed with Kapton tape for EXAFS measurements.

Figure 1. APT sample preparation locations in an irradiated UO2 fuel cross section.

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tom Probe Tomography affect microstructure include irradia- (APT) was performed to tion temperature, fission rate, fission Abetter understand defect density, and precipitation of fission and elemental composition of an products. Using a cross section of a

irradiated UO2 fuel sample. Focused commercial fuel pellet from Belgium ion beam, transmission electron Reactor 3 (BR3), APT tips were Atom probe tomography microscopy, and scanning electron created from a known radius location microscopy were assimilated together in the pellet. The locations of where to characterize the microstructure the APT tips were obtained can be of irradiated fuel provides of the UO2 fuel cross section. These seen in Figure 1. At the time of this techniques provide useful informa- report, the local irradiation parameters information on fission product tion that can be incorporated into of the APT location are unknown. fuel code models. By creating higher Twenty APT tips were prepared using accuracy models, the life time of fuel a Focused Ion Beam at INL’s Materials behavior in irradiated UO2 elements can potentially be extended. and Fuels Complex. Transmission This research supports the Office of electron microscopy of the APT tips fuels, which help support Nuclear Energy’s (DOE-NE) Light was performed prior to performing Water Reactor Sustainability (LWRS) APT analysis to compliment the APT Program and focuses on materials results. The APT tips were run using modeling efforts to extend integrity in the extension of the the CAMECA LEAP at CAES. Prelimi- lifetime of existing LWR fuels. nary results show that various fission fuel lifetimes in commercial products are present in the APT tips. Project Description Figure 2 shows a preliminary isocon- The purpose of this study was to centration surface of the UO focusing power reactors. perform APT of an irradiated UO 2 2 on Mo content. Figure 3 shows a 50 fuel sample to better understand the x 50 x 10 nm section of one APT tip defect and elemental compositional with isoconcentrations surfaces of — Brandon Miller, makeup of UO at various locations 2 other anticipated fission products. Mo in a fuel pellet. Inside a commercial Research Scientist, precipitates can be seen throughout UO2 fuel rod, the UO2 fuel will be Idaho National Laboratory the APT tips. Xe, Pd, Sr, and Y show under differing irradiation conditions increased concentrations at the loca- with various irradiation parameters tions of the Mo precipitates. Gd is an affecting the local microstructure. artifact in the APT results. Some irradiation parameters that can

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Figure 2. APT isoconcentration surface of Mo in the irradiated UO2 fuel.

Accomplishments Future Activities With little-to-no publications of APT Data analysis has commenced for the of irradiated fuels, this work provided project and a journal article will be first-of-a-kind data on behavior of created from the work once all data fission products in irradiated commer- has been compiled and the irradiation

cial UO2 at the atomic level. Under- history of the APT locations is finalized. standing fission product behavior in irradiated fuels supports modeling efforts and can potentially help extend the lifetime of commercial fuels, leading to increased efficiency of the current nuclear reactor fleet.

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Figure 3. APT isoconcentration surfaces of multiple fission products.

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Idaho National Laboratory Electron Microscopy Laboratory Collaborators Idaho National Laboratory Brandon Miller (co principal investigator), Mukesh Bachhav (collaborator) University of Florida Assel Aitkaliyeva (co principal investigator)

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In situ study of defect accumulation in Ti-6Al-4V under heavy ion irradiation: Influence of the microstructure and temperature Carl Boehlert – Michigan State University – [email protected]

ue to their high specific is known for the dependence strength, good fatigue and of its mechanical properties on This project investigates creep properties, corrosion thermomechanical processing. the irradiation damage D resistance, and commercial availability, Thermomechanical processing in Ti alloys for the titanium (Ti) alloys have been widely influences grain size and phase development of used in industrial, aerospace, and compositions. Improving the resistance engineering components biomedical applications. High compat- of materials to irradiation damage has for the Facility for ibility with coolants (e.g., lithium, been the subject of studies that focused Rare Isotope Beams helium, water) and low activation in on the effect of grain boundaries and at Michigan State radioactive environments also make grain size. The literature indicates that University. Ti alloys attractive for nuclear applica- a higher density of grain boundaries, tions. Specifically, Ti-6Al-4V(wt.%) was such as in nanocrystalline materials, selected to be a structural material for tends to exhibit a higher irradiation the beam dump in the Facility for Rare resistance. In addition, the effect of Isotope Beams (FRIB) at Michigan State the grain size on irradiation induced University (MSU). Limited studies have void formation was investigated in investigated the irradiation damage in copper and steel. Our study investigates these Ti alloys, specifically commer- the irradiation damage in Ti-6Al-4V cially available Ti-6Al-4V. Manufac- samples processed through two turing the complex shape of the Ti alloy different thermomechanical processes: FRIB beam dump presents difficult powder metallurgy (PM) rolled and challenges. Additive manufacturing additive manufacturing (AM). The constitutes an attractive alternative to latter was processed by direct metal casting and wrought processing due to laser sintering (DMLS) followed by hot its capability to produce near net shape isostatic pressing (HIP). As shown in components with less production time Figures 1 and 2, the samples exhibited and material waste. different microstructures. The PM rolled sample exhibited equiaxed -phase Project Description α grains, with the -phase typically One objective was to investigate the β present at grain-boundary locations effect of microstrucuture, dose, and whereas the AM sample exhibited a temperature on irradiation damage in lamellar + microstructure. This study titanium alloys. Both irradiation doses α β proposed to provide quantitative data and temperature affect the mechanical for the microstructural changes (defect properties of Ti-6Al-4V. Microstructure formation, defect clustering, defect evolution under irradiation at 25 and densities) and mechanical properties of 350°C induces different obstacles to these microstructures as a function of the dislocation motion. Ti-6Al-4V irradition dose.

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Figure 1. From upper left: (a) Backscattered electron scanning electron microscope photomicrographs and (b) electron backscattered diffraction inverse pole figures illustrating representative microstructures of the two studied as-processed Ti-6Al- 4V samples; 1) PM rolled and 2) additively manufactured

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Figure 2. Bright field TEM Accomplishments The AM microstructure exhibited a micrographs obtained at the IVEM– For this NSUF rapid-turnaround lenticular morphology of the + Tandem facility during irradiation for α β an additively manufactured Ti-6Al-4V experiment (RTE) project, we phases. The objective of this study alloy. The insets show the selected performed two different in situ was to evaluate the progression area diffraction patterns for the transmission electron microscopy of damage that occurs in Ti alloys central grain in the image. These irradiation experiments at the and to evaluate the influence of images show the progression of damage that occurred at the different Intermediate Voltage Electron microstructure on the damage fluences (indicated under the images) Microscope (IVEM)–Tandem Facility accumulation. For the 350°C which resulted from irradiation at at Argonne National Laboratory irradiation experiments, a relatively 450°C with 1MeV Kr ions. (ANL) with the assistance of the high dose of 24 dpa was achieved, following ANL staff: Dr. Meimei and transmission electron microscopy Li, Dr. Mark Kirk, Mr. Pete Baldo, bright-field images were acquired and Mr. Ed Ryans, and postdoctoral at different stages to show damage associate Dr. Jing Hu. During the first accumulation. The preliminary irradiation experiment at 350°C, qualitative results suggest that the we irradiated the two Ti-6Al-4V morphology of the α phase has alloys that underwent different an effect on defect accumulation. thermomechanical processing However, an in-depth evaluation of treatment. Their as-processed the crystal orientations of the α phase microstructures are shown in Figure in the irradiated areas has yet to be 1. The PM rolled microstructure performed and, thus, crystallographic exhibited an equiaxed α-phase effects cannot be ruled out. The morphology with the β-phase second irradiation experiment was decorating the grain boundaries. performed at 450°C on the same

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materials along with commercially structures and, in particular, establish Figure 3. Average hardness pure titanium (CP-Ti). We stopped whether dislocation loops were measured for the three different Ti samples irradiated at the Notre Dame the experiments at lower doses in formed in the α phase as a result of Tandem with 4 MeV Ar ions. Red order enable loop nucleation in the irradiation exposure, and if so, to symbols represent irradiated samples the α phase without the extensive characterize their density. while the black symbols represent the degradation associated with high unirradiated samples; solid symbols In addition to the aforementioned represent high dose rate (HDR, 13.4 dose rates that complicate such in situ irradiation experiments, we are dpa/hr) conditions while the empty analysis. Bright field TEM images investigating the effect of irradiation symbols represent the low dose rate were acquired in situ throughout both (LDR) (0.8 dpa/hr). exposure on the nanoindentation irradiation experiments. Figure 2 hardness for each of these materials. shows the evolution of irradiation We irradiated bulk samples using a 4 induced defects in an AM Ti-6Al-4V MeV Ar ion beam at both 25°C (i.e., sample irradiated up to 0.24 dpa room temperature[RT]) and 350°C. at 450°C. The nature of the defects This irradiation was performed using present has yet to be determined. the University of Notre Dame's 5U Post irradiation TEM characterization accelerator in collaboration with The of the irradiated CP Ti sample is Institute for Structure and Nuclear currently being performed as part Astrophysics (ISNAP) within the of an awarded NSUF proposal at the framework of the Radiation Damage Low Activation Materials Design and In Accelerator Target Environments Analysis (LAMDA) Laboratory at Oak (RaDIATE) collaboration. The samples Ridge National Laboratory (ORNL). irradiated at RT were exposed to The objective of this characterization two different dose rates, 0.8 dpa/h work is to determine the defect

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and 13.4 dpa/h, and reached the same final dose of 7.3 dpa within 1 µm of the surface. Nanoindentation measurements were carried out using an Agilent Technologies G200 nano indenter in collaboration with the LAMDA facility at ORNL. Figure 3 summarizes the nanoindentation hardness results for the six irradiated samples. We have observed that CP-Ti exhibited the highest irradiation induced hardening whereas the nanohardness of the AM Ti-6Al-4V was the most sensitive to the dose- rate effect. Focused ion beam (FIB) liftouts were extracted from the CP-Ti samples with the assistance of the researchers at the LAMDA facility at ORNL. TEM characterization is ongoing with the help of ORNL postdoctoral fellow Dr. Boopathy Kombaiah. Preliminary results are shown in Figure 4, displaying the evolution of defects as a function of depth in the CP-Ti sample irradiated at the lower dose rate. Future Activities Further investigation and TEM characterization is ongoing at the LAMDA facility to understand the different damage structures in irradiated Ti-alloy samples at different doses. The results from the TEM and nanoindentation characterization of the irradiated Ti alloy will be published. As discussed previously, the microstcutures of the Ti-6Al-4V alloys Figure 4. (a) Low magnification and (b) high magnification TEM bright field micrographs of the same area of a CP-Ti sample after irradiation at RT with 4 MeV examined were significantly different Ar ions at LDR of 0.8 dpa/hr. Both arrows indicate the direction of the Ar ion beam due to the different processing and the arrow in (a) points to the border between the platinum layer deposited on methods utlized. The PM rolled sample the surface which was used to assist the FIB lift out. exhibited equiaxed α-phase grains with the β-phase typically present at grain boundary locations whereas the AM sample exhibited a lamellar

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Figure 5. Picture of the ANL IVEM in use during in situ ion irradiation experiment.

The IVEM facility provides unique capabilities α+β microstructure. Future work have qualitatively shown the defect is intended to provide quantitative accumulation during irradiation and to investigate, in situ, data for the microstructural changes we now need to measure the defect (defect formation, defect clustering, densities as a function of irradiation defect densities) and mechanical dose and time and temperature. the evolution of ion properties of these microstructures as a function of irradition dose. We irradiation damage.

Distributed Partnership at a Glance — Aida Amroussia, NSUF and Partners Facilities and Capabilities PhD Graduate student Argonne National The Intermediate Voltage Electron Laboratory Microscopy (IVEM)–Tandem Facility Collaborators Argonne National Meimei Li (collaborator) Laboratory IVEM – Tandem Facility Michigan State University Aida Amroussia (co principal investigator), Carl Boehlert (principal investigator) National Superconducting Frederique Pellemoine (collaborator), Cyclotron Laboratory Wolfgang Mittig (collaborator) (NSCL) - Facility for Rare Isotope Beams (FRIB)

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Irradiation effect on the heterogeneous hardening of cast austenitic stainless steels Wei-Ying Chen – Argonne National Laboratory – [email protected]

Figure 1. EBSD map shows the morphology of a CASS CF 8 where the yellow matrix is the austenite phase and the red islands are the ferrite phase.

ast austenitic stainless steels ment and neutron irradiation (CASSs) are structural mate- damage; these phenomena are of Crials used for components concern after long-term exposure at the primary pressure boundaries to reactor core environments. In and core internals of light water this project, we investigated the reactors (LWRs). Consisting of a embrittlement of CASS subjected dual-phase microstructure of delta to neutron irradiation and thermal ferrite and austenite, as shown in aging treatment. The delta ferrite Figure 1, CASS alloys are suscep- and austenite behave very differ- tible to thermal aging embrittle- ently under thermal and neutron

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Figure 2. Dark field TEM images of the ferrite and austenite phases in CASS after thermal aging and neutron irradiation. The yellow text boxes summarize the microstructural characteristics observed by TEM and APT.

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Figure 3. The hardness of exposure. Therefore, to understand characterization and nanoindenta- the ferrite and austenite the embrittlement mechanism in the tion, we showed that the ferrite phase in CASS from nanoindentation in the dual phase microstructure of CASS, and austenite respond differently to unit of GPa. the hardening in delta ferrite and thermal aging treatment and neutron austenite need to be investigated irradiation, leading to an inhomo- separately. However, the thin shape geneous development of hardness of delta ferrite (a few microns in in two phases, which is critical width) poses difficulty in traditional for the deformation of dual phase microhardness measurement. microstructures and is contributing to the embrittlement of CASS alloys With nano indentation measure- in service. The outcome of this study ments, we were able to measure the will help develop a scientific basis hardness evolution of delta ferrite for assessing and managing the and austenite individually with a fine embrittlement of CASS components scale. Combining the microstructural under LWR service conditions.

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Project Description results were compared with the In this project, we used nanoindenta- microstructural characterization tion to measure the hardness of the using transmission electron micros- delta ferrite and austenite in a number copy and atom probe tomography of CASS CF3 and CF8 after thermal (APT) to understand the relation aging and neutron irradiation. The between microstructural modifica- The unique capability of laboratory aging was performed at tion due to irradiation and thermal 400°C for 10,000 hours. The irradia- aging on the mechanical property tion was performed in Halden reactor of the delta ferrite and austenite in nanohardness measurement at 320°C to a dose of 0.08 dpa. The CASS. This work provides detailed specimens were all in the shape understanding on the heterogeneous of 3 mm discs with a thickness of evolution of microstructure and on radioactive materials about 200 µm. The specimens were mechanical property in CASS under electropolished to remove the surface the extreme conditions of nuclear enables the study on materials deformation, and then mounted on reactors and serves as a stepping SEM stubs using superglue. stone for developing a model to describe large scale mechanical of complex structure for use Nanoindentation was performed in properties such as fracture tough- the Microscopy and Characterization ness, enhancing the ability to predict Suite in the Center for Advanced under the extreme conditions the long-term stability of CASS in Energy Studies (CAES). The delta nuclear reactors for an extended ferrite and austenite phase were service life of 60 years. of nuclear applications indented, each with multiple indents for good statistics. The hardness — Wei-Ying Chen,

Table 1. List of specimens examined Postdoctoral Researcher

Materials Pre-irradiation Aging Irradiation CF3 unaged 0.08 dpa CF3 400°C 1000 hours 0.08 dpa CF8 unaged 0.08 dpa CF8 400°C 1000 hours 0.08 dpa CF3 unaged No irradiation CF3 400°C 1000 hours No irradiation CF8 unaged No irradiation CF8 400°C 1000 hours No irradiation

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Accomplishments conditions. Dislocation loops cannot be evidently observed in the ferrite The long-term We have successfully achieved the phase after neutron irradiation. degradation of cast goal of the proposed scope to obtain the individual hardness of the delta austenitic stainless steel By contrast, in the irradiated austenite ferrite and austenite in duplex (CASS) is an important phase, some dislocation loops can be CASS of various thermal aging and issue for light water observed along with the formation of neutron irradiation conditions, and reactor sustainability. the precipitates enriched in nickel and to correlate the hardness to the This project is the silicon. However, the total density of microstructures previously char- first reported study to dislocation loops and precipitates was acterized with TEM and APT. TEM use nanoindentation very low, so hardness did not increase. characterization was performed in to obtain the Thermal aging alone did not cause the Intermediate Voltage Electron heterogeneous microstructural modification in the Microscope (IVEM)-Tandem Facility hardening in CASS as a austenite phase and, therefore, did not in Argonne National Laboratory. result of thermal aging change the hardness. The irradiation Zhangbo Li from the University of and neutron irradiation. and thermal aging effects were quali- Florida carried out APT in CAES. tatively the same for CF3 and CF8. As shown in Figure 2 and Figure 3, hardness and the microstructure can Future Activities be consistently correlated. The ferrite We will continue this work by experienced considerable hardening studying the same set of CF3 and (roughly 40% more) after thermal CF8 CASS that had been neutron- aging as well as neutron irradiation irradiated to 3 dpa, a higher dose due to the formation of G-phase than the present study. Preliminary precipitates and spinodal decomposi- TEM examinations show that the tion. The microstructures resulting austenite phase accumulated irradia- from neutron irradiation and thermal tion damage in the form of a high aging were similar, leading to a density of faulted dislocation loops comparable degree of hardening in while the ferrite phase seems to spite of their distinct experimental exhibit similar microstructure as its 0.08 dpa counterpart. We plan to use nanoindentation to investigate the heterogeneous hardening in these 3 dpa CASS specimens.

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Publications Cast Austenitic Stainless Steels,” [1.] Y. Chen, W.-Y. Chen, B. Alexan- Proceedings of the 18th Inter- dreanu, K. Natesan and A.S. Rao, national Conference on Environ- “Crack Growth Rate and Fracture mental Degradation of Materi- Toughness of CF3 Cast Stainless als in Nuclear Power Systems Steels at ~3 DPA,” Proceedings – Water Reactors, August 13-17, of the 18th International Confer- Portland, OR. ence on Environmental Degra- [3.] W.-Y. Chen, Y. Chen, Z. Li, C. Xu, dation of Materials in Nuclear Y. Yang, N. Demas, “Effects of Power Systems—Water Reactors, thermal aging and neutron irra- August 13-17, Portland, OR. diation on Cast Austenitic Stain- [2.] Y. Chen, C. Xu, X. Zhang, W.-Y. less Steels,” TMS Annual meeting, Chen, J.-S. Park, J. Almer, M. San Diego, CA 2017. Li, Z. Li, Y. Yang, A.S. Rao, B. Alexandreanu and K. Natesan, “Microstructure and Deforma- tion Behavior of Thermally Aged

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Argonne National Wei-Ying Chen (principal investigator), Laboratory Yiren Chen (co principal investigator) University of Florida Yong Yang (co principal investigator)

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Wigner Energy of SiC irradiated to high levels of swelling Lance L. Snead – Massachusetts Institute of Technology – [email protected]

Figure 1: High resolution hile stored energy is well driving an autocatalytic temperature TEM Image of highly understood conceptually rise. However, recent work on the defected SiC sample Wand has been studied gross swelling of silicon carbide has in detail for gas-cooled reactors, suggested significant Wigner energy the Szilard Complication has been in another important nuclear mate- generally and practically thought rial (SiC) system may exist. (Snead to be unique to graphite. In other et al. JNM 471 [2016], 92–96) In words, for practical nuclear systems this project, the Wigner energy in the combined stored (Wigner) highly defected, neutron irradiated energy due to simple production SiC is determined and compared with is only an issue for graphite irradi- physical swelling and lattice dilation. ated <200°C, where the subsequent The extended goal of this research energy release upon annealing greatly is to provide a full understanding of exceeds the materials’ specific heat, the SiC annealing kinetics irradiated

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at low to intermediate irradiation PC-3-M3(0.05 × 1025 n/m2), temperatures to judge whether PC-4-M4(2 × 1025 n/m2), and Wigner energy could be an issue for PC-5-M5(20 × 1025 n/m2). Addition- the use of SiC at the relatively low ally, an opportunity to piggyback temperature applications currently upon a set of irradiation vehicles of under consideration. similar design (i.e, perforated HFIR rabbits) became available and was Project Description exploited. Specifically, Dr. Terrani The technical objectives for this arranged for space in a critical amor- project are two-fold. The first is Similar to the well-known phization transition range. Data were the practical point of answering if Wigner Energy release also obtained on swelling at 0.762 Wigner energy exists in SiC to an in irradiated graphite, and 1.34 × 1025 n/m2, also at 90°C. appreciable amount, meaning can for the first time this In addition to the PI, the research energy be stored and released such work demonstrates a team included Wally Porter, Takaaki that an autocatalytic reaction takes significant energy Koyanagi, Yutai Katoh, and Kurt place. Information on such a reaction release in a second Terrani at ORNL. Energy release was would clearly be of concern for and important nuclear carried out using a Netzch 404C DSC necessary to reactor designers, which material, specifically within the Low Activation Materials may be of increasing importance silicon carbide. Development and Analysis (LAMDA) as SiC is now being considered for laboratory at ORNL. Supporting x-ray lower temperature applications and transmission electron microscopy (e.g., LWR cladding) as opposed were also carried out to provide to the historic HTGR applica- insight into the microstructure, tion. In order to address this first also in LAMDA. point, a bounding set of materials was selected that would provide a Accomplishments maximum Wigner energy. The second In a previous paper by the goal of this work is to provide some author (Snead et al. 2016) an fundamental and quantitative under- extraordinary level of swelling standing of the process to help guide prior to amorphization in SiC was future research. This was accom- observed: ~8% lattice expansion plished by combining Wigner energy as measured by x-ray and density as measurements with the study of measured by density gradient column. underlying microstructural evolution. By straightforward calculation, assuming the annihilation of vacancies The experimental approach was of ~5eV per vacancy-interstitial conceptually simple, taking advantage of recombination, the restoration of high purity CVD SiC utilized in previous the SiC structure through annealing irradiation capsules irradiated in the would liberate ~1875 J/g. This High Flux Isotope Reactor. The specific suggests an energy release on the designation of the historic samples were order of ~1.5 J/g-K as compared PC-1-M1 (0.02 ×1025 n/m2), to an average specific heat for SiC PC-2-M2(0.1 × 1025 n/m2),

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Figure 2: Swelling and energy release of irradiated SiC samples

(RT-700°C) of under ~1 J/g-K. Given An example of the highly defected this, it is a reasonable possibility structure is shown in Figure 1 for a that low-temperature irradiated highly pure CVD SiC material that SiC could have a Wigner energy underwent 7.7% swelling. Of interest release exceeding the specific heat is that the material has a large lattice and, therefore, leading to a positive strain due to the accumulation of temperature excursion. The primary irradiation induced defects. While the goal of this work was to directly material clearly has remained crystal- measure the energy release in such line, as evidenced by the diffraction highly defected, highly strained pattern, discontinuous pockets of very material to scope the magnitude of highly damaged areas that approach the stored energy and rate of energy amorphous materials are appearing. release in comparison with specific From the annealing literature, it is heat. An important secondary goal known that an approximately linear was to gain understanding of the annealing curve behavior takes place underlying microstructure of the in highly defected SiC with near material in the irradiated and annealed complete annealing at or just above material to guide future experiments. 1000°C. For this reason, it would be expected that a large number of

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the defects would annihilate upon The primary technical goal of iden- high temperature annealing. Figure 2 tifying whether significant Wigner provides results to date on irradiation energy exists in SiC in any appreciable induced swelling, swelling recovery, amount has been unambiguously and Wigner energy release for the demonstrated and for these irradiation irradiated CVD SiC samples of this conditions is clearly appreciable. It is study (in this experiment, we were noted that the irradiation conditions limited to 700°C annealing). From for executing this rapid turnaround the figure, the swelling of the SiC is experiment were chosen to provide seen to follow a linear swelling with maximum Wigner energy, and were dose achieving a maximum of 8.13% for lower temperatures than LWR volumetric expansion. The maximum cladding or other currently conceived energy release is 1390 J/g-K with a advanced reactor applications of SiC. possible extrapolation to on the order In this light, a future, more compre- of 2000 J/g-K. This amount of energy hensive survey of Wigner energy for release, as discussed notionally above, is SiC as a function of irradiation and in excess of that necessary for a positive temperature would be prudent. temperature excursion in SiC. As seen Future Activities in the figure, above this dose and prior This rapid turnaround experiment to the dose of 1.34 × 1025 n/m2 (E has provided the first direct evidence >0.1 MeV) the crystal makes a transi- of appreciable Wigner energy in SiC, tion from crystalline to amorphous, albeit at temperatures lower than of achieving a maximum volumetric general interest to nuclear applica- expansion of ~11.7% (2.84 g/cm3). tions. Follow-on work is suggested. Above the critical amorphization dose, the energy release substantially Publications decreases, consistent with the notion To be published of the material making a transition to a lower energy state.

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In Situ observation of lunar-crater features in

Xe irradiated UO2 at high dose Lingfeng He – Idaho National Laboratory – [email protected]

Figure 1. (Left) Argonne-IVEM o simulate fission fragments ysed using dark field imaging, high for in situ TEM observation damage and fission gas evolu- resolution TEM imaging, energy of UO2 irradiated with 300 eV Xe. (Right) SRIM calculation Ttion in UO2, the 300 keV Xe dispersive x-ray spectroscopy (EDS), showing the radiation damage ion beam in the Intermediate Voltage and energy-filtered TEM techniques. level (dpa) and Xe concentration Electron Microscope (IVEM)–Tandem Small Xe bubbles were investigated 16 2. at 5 × 10 ions/cm facility at Argonne National Labora- by the underfocus and overfocus tory (ANL) was used to irradiate image techniques. polycrystalline UO lamella. The 2 Project Description damage depth is around 150 nm, Uranium dioxide (UO ) is the most which is close to the thickness of 2 widely used nuclear fuel in commer- UO lamella and good for in situ 2 cial light water reactors. The cumula- observaton by transmission electron tive radiation damage during the microscopy. This rapid turnaround fission process causes severe degrada- experiment revealed the nucle- tion in the thermophysical properties ation and evolution of lunar-crater of UO fuels, which limits their features in UO as a function of 2 2 lifetime and increases their opera- irradiation dose and temperature. tional cost. Therefore, investigating The compositon and microstructure both defect production and evolution of lunar-crater features were anal- and fission product transport under irradiation to reveal their physical

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Figure 2. Lunar-crater feature evolution at 600°C as a function of dose (lunar-crater features occur at 280 dpa).

mechanisms is of great importance will shed light on both the dose and in understanding the degradation of temperature effects on lunar-crater

thermophysical properties of UO2 features formation and evolution. fuels. In this work, both in situ and Further, the experimental microstruc- ex situ TEM observation of defect nucle- ture characterization will provide a ation and evolution under ion irradia- fundamental foundation for atomic- tion was conducted to understand the level modeling, which is conducted at radiation damage mechanisms in UO2 Idaho National Laboratory and Purdue at high damage levels. The irradiation University. This marks the first creation

induced microstructure, including of lunar-crater features in UO2. In situ dislocation loops, inert gas bubbles, studies of crater feature formation and

and lunar-crater features are character- evolution in UO2 using the IVEM- ized using state-of-the-art character- Tandem facility provides a unique ization tools. Revealing the nucleation opportunity to study the effects of and evolution of lunar-crater features bubble pressure on microcracking,

at high dose is the main purpose of blistering, and exfoliation in UO2. this study. The comparison between Our work has contributed to DOE’s

the microstructure features of UO2 leading role in basic science research under various doses and temperatures

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Figure 3. Lunar-crater feature of materials behavior and performance 25°C, at a dose of 280 dpa at 600°C, evolution as a function of in extreme environments. In addition, and at a dose of 252 dpa at 800°C. irradiation temperature (lunar- crater features occur at higher the microstructural characterization An extensive study on the chemical dose at lower temperature). and modeling of radiation effects on analysis using ChemiSTEM indicates

UO2 can guide the design of next the crater features are slighly rich in generation nuclear fuels. Xe compared to the matrix. Accomplishments The formation mechanism of lunar The microstructure evolution under crater features has been extensivly

high dose irradiation in UO2 is not discussed. Xe-implantation induces yet well understood. The IVEM – various types of defects, such as inter-

Tandem Facility at Argonne National stitials and vacancies in UO2. Vacancies Laboratory was employed to study act as efficient trapping centers for the defect evolution in Xe irradiated the implanted Xe and turn into Xe

UO2 at high dose (Figure 1). In situ bubbles after trapping Xe (Figure 4). TEM observation shows that the The implanted Xe segregates into formation of crater featues depends bubbles, which thereby create internal on the ion dose and irradiation pressure and reach an overpressur- temperature (Figures 2 and 3). The ized state. When this internal pressure

higher the irradiation temperature, attains the fracture limit of UO2, it the lower the dose at which the ultimately lifts the implanted surface lunar-crater featues occur. The crater in the form of surface blistering and features occur at a dose of 315 dpa at exfoliation and generates lunar-crater

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features in UO2. The formation of The implanted layer developed a Figure 4. TEM images of lunar-crater features depends on both structure of small crystallites, which bubbles in UO2 irradiated with 300 keV Xe ions at 600°C up ion dose and temperature.The bubble were misaligned by a few degrees. The to a dose of 5 × 1016 ions/cm2. pressure at high temperature is higher transformation could be produced at (a) is an overfocus image, and than that at low temperature, which 77 K, room temperature, and 500°C (b) is an underfocus image. The bubble size and density are makes the blistering and exfoliation in the same dose range. The dose level, 23 -3 2.3±0.3 nm and (8±4)×10 m , occur at lower dose. However, the Xe ion energy, and irradiation temper- respectively. detailed mechanisms of the surface ature in the present study are compa- blistering and exfoliation are very rable to those in Matzke’s work. The complicated and more efforts are round features, therefore, could be the needed to understand them. sign of the starting polygonization. HRTEM work by Matzke and Wang Matzke et al. investigated radiation revealed the formation of subgrain effects in UO under high dose Xe 2 boundaries in Xe irradiated UO up implantation by ion beam techniques 2 to a dose of 5 × 1015 ions/cm2, and (Rutherford backscattering and chan- the small subgrains of nanometer neling) and found a critical dose typi- size were slightly rotated (about 1–2 cally around 3 to 5 × 1016 ions/cm2 degrees with respect to one another for the formation of a “polygonization across the sub grain boundaries) peak” in single crystal UO2 (Nuclear Instruments and Methods in Physics Research B 91 [1994] 294-300).

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Figure 5. Lunar-crater features in Xe irradiated UO2 at a dose of 350 dpa and 600°C. (a) low magnification and (b) high magnification STEM images; (c) TEM image; and (d) EFTEM image showing the thickness map of (c).

(Journal of Nuclear Materials 231 tracks that may divide large grains. [1996] 155-158). These irradia- However, the direct evidence of the tion induced nano subgrains could latter two mechanisms from TEM is be the nuclei for polygonization still lacking. The size and density of

in UO2, but the critical dose of the the round features are also influenced subgrain formation is one order of by the foil thickness. Defects and Xe magnitude lower than that for the ions are more prone to accumulate formation of polygonization peak at the thick foil regions as compared and the round features found in this to the thin foil regions because the work. Alternatively, polygonization Xe out-diffusion is hindered and the may also be induced by the overpres- surface cannot efficiently annihilate surized bubbles. The bubbles may the irradiation defects. Thus, the high cause cleavages and cracks on a very strain due to Xe build up and damage small scale, as well as amorphous at the thick region may contribute to the formation of the observed round features.

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This experiment will clarify the radiation damage

mechanisms of UO2 under ion irradiation at high dose. The IVEM is a powerful

Future Activities and more efforts coupling experi- instrument offering Future goals for this research ments and computation are needed include simulating the nucleation to clarify the mechanism. and evolution of lunar-crater in situ observation of defect Publications features in UO under irradiation 2 [1.] L. He, X.M. Bai, J. Pakarinen, B. and bettering the understanding of Jaques, J. Gan, A.T. Nelson, A. nucleation and evolution formation mechanims. Lunar-crater El-Azab, and T.R. Allen. “Bubble features may also form in other Evolution in Kr-irradiated UO materials, and in situ observation of 2 under irradiation during Annealing,” J. Nucl. Mater. formation and evolution of these 496 (2017), pp. 242–250. features in other materials is worthy of further investigation. The grain [2.] L. He, J. Gan, M. Kirk, B. Tyburska- — Lingfeng He, boundary effects on the formation Pueschel, B. Jaques. “Radiation Senior staff scientist of lunar-crater features could be of Damage on UO2 and UN,” TMS importance, and further study is also 2017 Annual Meeting & Exhibi- needed. The polygonization mecha- tion; Feb 26-March 2, 2017, San nism in UO2 is still under debate, Diego, California, USA (Invited).

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Argonne National The Intermediate Voltage Electron Microscopy Laboratory – Tandem Facility Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Argonne National Marquis A. Kirk (collaborator) Laboratory Idaho National Laboratory Jian Gan (collaborator), Lingfeng He (principal investigator)

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Investigation of the interface strength for matrix-fiber interface of irradiated SiC composite materials Yutai Katoh – Oak Ridge National Laboratory – [email protected]

iC/SiC composites exhibit specimens by preparing micropillars exceptional high-temperature using scanning electron microscopy/ Sstrength and radiation-resistant focused ion beam (FIB) and in situ flat- properties, making them an advanta- punch compression testing via nano geous choice for accident-tolerant indentation. With a comprehensive nuclear fuel cladding. The composite and fundamental understanding, the architecture allows an intrinsically property data and associated impact brittle material to exhibit sufficient on mechanical behavior could be SiC/SiC composites structural toughness. This study implemented into a predictive model, push the boundary evaluates the importance of the fiber/ improving safety and reliability for for operational matrix interphase as it relates to accident tolerant fuel. Establishing this performance in extreme composite toughening mechanisms. new state of knowledge has significant environments. Detailed Small-scale mechanical testing along impact on academic theory of ceramic characterization with atomic-force and transmis- composite toughening mechanisms, and experimental sion electron microscopy analyses as well as industrial application based understanding of have been employed to evaluate component design. Macroscopic interface properties PyC interphase properties that play failure analysis has led to linear elastic will enable a key role in the overall mechanical fracture models that describe the microstructurally behavior of the composite. The Mohr- role of the interphase in micro-crack informed models for Coulomb failure criterion allowed for deflection. However, experimental improved engineering the extraction of an internal friction validation of these physics models predictability. coefficient and debonding shear has not been fully exhausted. Micro- strength as a function of the PyC layer pillar compression allows for a more thickness and irradiation. intrinsic understanding of interface properties and is expected to aid Project Description in theory validation. For industrial The technical objective of this research application, traditional homogenized is to use experimental techniques to composite modelling techniques can investigate the change in fiber-matrix implement these extracted property interphase properties for irradiated data directly. In this manner, the effects SiC/SiC composite materials. In of irradiation on interphase-dependent particular, the focus is on evaluating mechanical behavior may be system- ultimate shear strength and fric- atically explained. This will result in tion properties in the irradiated design improvement which can be implemented to enhance composite

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Figure 1. A typical 3 µm micro- pillar structure undergoing in situ compression test. The stress state and force balance that are used to extract debond shear strength and internal friction values are overlaid.

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Figure 2. Extraction of the debond shear strength (intercept) and internal friction coefficient (slope) by application of the Mohr-Coulomb fracture criterion that plots the resolved shear stress versus the resolved normal stress at failure.

performance in neutron irradiation of this research required strong environments and will thereby support cooperation and communication the mission of DOE-NE for reliable and between all participants for handling efficient nuclear power systems. and evaluation of the irradiated specimens. Takaaki Koyonagi of ORNL Accomplishments was a quick and reliable correspon- The technical goal of this research was dent with attention to detail. He was to compare pristine and irradiated responsible for obtaining, tracking, and interface property data via micro-pillar communicating the expectations for compression. This goal was achieved the pre-irradiated SiC/SiC composite through refinement of micro-pillar samples. With access to state-of-the-art fabrication, increased sampling size, facilities, he was also able to polish and application of the Mohr-Coulomb the irradiated samples prior to ship- Mohr failure criterion. As the project ment to UC Berkeley, which simplified moved forward, it quickly experienced work for the university and allowed success and additional samples with for expedited results. In total, two variable PyC interface thicknesses pristine control samples, two irradiated were also received, allowing for more samples, and one thick PyC interface thorough understanding of interface sample were obtained by Oak Ridge design space. Pragmatically, the goals National Laboratory, followed by

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interface analysis at UC Berkeley. All When samples are tested in compres- samples contained HNLS nuclear grade sion, the Mohr-Coulomb criterion fibers. Sample A and A_rad exhibited describes the stress state at failure with five alternating layers of PyC/SiC equation 1: before full CVI SiC infiltration, while sample B and B_rad were fabricated (P break * sinθ) (P break * cosθ) = τdebond + *μ (1) to have a single monolayer of PyC at A A the fiber surface. Sample C exhibited a monolayer PyC interface ~1300 nm allowing for the extraction of thick. Sample A_rad received 0.97 dpa τdebond and μ. For each test, the failure load at 300°C, and sample B_rad received (P ) was extracted from the load 11.8dpa at 280°C. break vs displacement curves and used to The availability, preparation, The primary technique applied in this calculate the resolved normal stress research was micro-pillar compres- and resolved shear stress during and testing of the irradiated sion. Compared to fiber push out failure, at the failure plane. Each testing, micro-pillar structures can sample yielded data for its respec- SiC/SiC samples has expanded offer refined property extraction τ( debond tive incline plane, which these data and µ), interface characterization, and were then plotted. Applying the consistent trials. Focused ion beam Mohr-Coulomb criterion allowed us and enriched the content of my (FIB) milling techniques were used to understand how the contributing to fabricate the micro-mechanical debond resistance properties were structures. Pillars (~3 µm in diameter) evolving as a function of irradiation. PhD thesis. I’m grateful for were fabricated with a fiber/matrix In Figure 2, we plot the resolved interphase spanning its cross-section. shear stress versus the resolved this opportunity to collaborate. All milling processes followed a similar normal to apply a linear fit, for which cutting sequence with a rough cut the slope is equivalent to the internal (10–15 nA) followed by finishing cuts friction coefficient and the intercept — Joey Kabel, (0.1–0.5 nA). Once fabricated, the equivalent to the chemical debonding Graduate Student Researcher pillars were tested in situ with the SEM stress. Table 1 summarizes the and Hysitron PI-85 Pico Indenter using extracted properties. a 5 μm flat punch diamond tip, with displacement controlled loading at 10 nm/s. The experimental work and data analysis were primarily carried out by UC Berkeley graduate student Joey Kabel. Figure 1 shows a representative micro-pillar structure and overlaid stress state during failure.

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Figure 3. TEM foil lift out of the fracture pillar with PyC interface. The TEM analysis showed failure occurred within the PyC structure, suggesting properties are dependent on PyC structure.

TEM analysis of failed pillar interfaces, graphite-like basal plane alignment/ Figure 3, revealed that failure was long range order for increased deposi- occurring within graphite-like struc- tion thickness, and decreased long range ture of the PyC interface, suggesting order during irradiation. Another influ- that extracted properties are inherent to ence was the significant non-uniform the deposited PyC. porosity that evolved in the 11.8 dpa sample, shown in Figure 4. It can be observed that while the chemical debonding strength decreases It is believed that this porosity is respon- with irradiation, the friction coefficient sible for the low statistical confidence appears to increase. With respect to in the extracted properties. However, thickness, both the debond strength and the trend of increased internal friction internal friction coefficient are observed and decreased strength is still observed, to decrease. This may be a result of likely enhanced by the porosity.

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Figure 4. Observation of PyC interface degradation at 11.8 dpa sample irradiated at ~260–280°C. These high dose pillars showed increased internal friction and decreased debond shear strength.

Internal friction Fiber τdebond (MPa) coefficient (µ) Successful tests A (50nm PyC) 266 ± 23 0.25 ± 0.03 17 B (100nm PyC) 158 ± 19 0.22 ± 0.06 11 C (1300nm PyC) 133 ± 14 0.17 ± 0.03 8

Arad (0.97 dpa) 103 ± 11 0.36 ± 0.03 16

Brad (11.8 dpa) 37 ± 59 0.89 ± 0.20 7

In conclusion, micro-pillar Future Activities compression was implemented to In the final month of 2017, continued examine the interface properties data analysis and write up (for both of SiC-SiC composite interphases journal submissions and conference as a function of irradiation and procedings) are expected. Future thickness. SEM and TEM observations goals for this project may include revealed insight into interface failure a more rigorous TEM analysis and mechanisms and irradiation damage, understanding of PyC degradation and providing some explanation of the falure mechanisms as a funciton of observed PyC property evolution. dpa and thickness. It is also expected

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Figure 5. Joey Kabel (graduate student) trains Ruijie Shao (undergraduate student) on micro-pillar fabrication techniques using FEI Quanta dual beam FIB at the University of California, Berkeley Nuclear Materials Laboratory, an NSUF Partner Facility.

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that increasing the number of pillars of SiC-SiC Composite Interphase tested, especially for the 11.8 dpa Properties and Debond Mecha- sample, will increase statistical fidelity nisms J. Kabel,” Compos. Part B and improve confidence in property Eng., vol. 131, pp. 1–18 (Else- implementation into finite element vier), 2017. models. Another step forward would [2.] J. Kabel, P. Hosemann, Y. Zayachuk, be to characterize the mode I frac- D. E. J. Armstrong, T. Koyonagi, ture release rate energy as it applies Y. Katoh, C. Deck. “Ceramic directly to understanding limitations fiber-matrix composite interface and interface design optimization property evaluation and testing on for microcrack deflection. We believe SiCf / PyC / SiCm composites.” J. the collaboration has been successful Mat. Res. and are excited to continue our work through additional proposals and [3.] J. Kabel, M. Balooch, Y. Yang, T. utilization of the Nuclear Science Koyanagi, K. A. Terrani, P. Hose- User Facilities. mann. “SiC-SiC Composite Inter- phase Evaluation via Small Scale Publications Mechanical Testing.” American [1.] J. Kabel, Y. Yang, M. Balooch, C. Nuclear Society. Winter Meeting Howard, T. Koyanagi, K. A. Ter- 2016; Las Vegas USA. rani, Y. Katoh, and P. Hosemann, “Micro-Mechanical Evaluation

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities University of Nuclear Materials Laboratory California, Berkeley Collaborators Oak Ridge National Takaaki Koyanagi (collaborator), Laboratory Yutai Katoh (principal investigator) University of Joey Kabel (collaborator), California, Berkeley Peter Hosemann (collaborator)

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A TEM study of proton, heavy-ion and neutron irradiated FeCr Steve Roberts – University of Oxford – [email protected]

Figure 1: From left to right: he main focus of this project complex, long, and expensive, with SEM image of the grain is to investigate the extent to very little freedom to control the structure; FIB lift out produced with two “windows” to Twhich surrogate irradiations irradiation parameters. The alternative reduce foil bending and TEM by protons and heavy ions can be is to irradiate samples with charged image of typical unirradiated used to reproduce the microstructural particles such as heavy or light ions microstructure. and mechanical changes brought on or electrons. Charged particles allow by neutrons in ferritic-martensitic greater control over irradiation (FM) materials. parameters, little or no radioactivity induced into samples, and far less Reduced activation ferritic-martensitic time required to reach a particular (RAFM) steels are promising materials dose. In order to validate the use of for structural components and more such surrogate particles, they must be accident tolerant fuel clad consid- directly compared with neutron irra- ered for future fission devices. Their diation under matching conditions. advantages include reduced swelling compared to austenitic steels and Radiation damage is highly depen- no long term induced radioactivity. dent on the chemical composition To predict their performance in a of a material. Complex RAFM steels, working reactor, the effects of neutron such as T91, have many elements damage on RAFM materials must which complicate the analysis of be tested and understood. Fission the radiation damage and compari- reactors are the closest analogue sons with other steels. In order to currently available to test materials in understand radiation damage in such the radiation environment expected steels, it is essential to understand the within such advanced nuclear devices. radiation damage in simpler alloys. However, such experiments are Therefore, this project studies binary alloys of FeCr.

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Highlighting the differences among neutron, proton and self ion irradiation is crucial to understanding and interpreting irradiation experiments that attempt to mimic reactor conditions with charged particle beams.

Project Description In order to achieve the objectives of The objective of this work was to this project, access to a facility capable compare the microstructures of of handling radioactive neutron proton, heavy ion, and neutron irradiated samples was required. irradiated FeCr binary alloys. Alloys Neutron irradiated materials were of Fe6Cr and Fe9Cr were selected for produced in the University of their particular relevance to candidate California at Santa Barbara (UCSB)- RAFM steels. Of particular interest Advanced Test Reactor (ATR) 1 were the dislocation loops and cavities irradiation campaign, carried out by that can be produced during irra- Robert Odette in 2009. The materials diation, and also changes (if any) to originated from capsule 1A of this chromium distribution in the alloys. experiment. Since the irradiation experiment, these materials were The neutron irradiated alloys studied stored at Idaho National Laboratory in this work are of considerable (INL) to allow radioactivity to reduce. relevance to the development of The alloys were irradiated to ~1.8 dpa RAFM steels as they will improve at 288°C over 200 days. The focused our understanding of the role ion beam (FIB) microscope at the chromium has in the evolution Center for Advanced Energy Studies of microstructural defects during (CAES) was used to prepare lift outs irradiation and subsequent radiation for transmission electron microscopy induced hardening. Understanding on each of these alloys. The CAES these mechanisms is invaluable to facility was ideal for this work because the development of new RAFM steels. of the experience of CAES and INL Furthermore, comparisons to proton staff with working on active material and heavy ion irradiation damage and close proximity to INL. will lead to improvements in the design of irradiation experiments that use charged particles to replicate reactor conditions.

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Figure 2. Neutron irradiated Accomplishments Weak-beam dark field (WBDF) Fe9Cr microstructure. Dark field FIB lift outs were prepared initially imaging in the TEM has shown the micrograph is shown with inverted contrast. Figure shows the at CAES before being shipped to the neutron irradiated Fe9Cr micro- pre-existing screw dislocations UK, where final thinning of the TEM structure contains dislocation loops, transformed into helices with foils was conducted (Figure 1). It was which form from the point defects a locally high population of important to prepare the samples in produced after collision cascades. Both dislocation loops. this two-stage process in order to 1/2<111> and <100> Burgers vector minimize the time between foil- dislocation loops were found in the thinning and analysis in the TEM. material, which can both cause hard- Successful sample preparation has ening in the material by impeding been completed for both Fe6Cr and dislocation motion. The defects have a Fe9Cr alloys. highly heterogeneous spatial distribution in the grains; the majority of Ion irradiation and proton irradiation dislocation loops are found decorating of the same materials has also been dislocations that existed prior to conducted to match the dpa dose and irradiation (Figure 2). temperature of the neutron irradiated material as closely as possible.

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The microscopes and personnel at the CAES facility are world class when it comes to working with active material, and the close ties with INL were invaluable.

— Jack Haley, Co Principal Investigator

Figure 3. Ion irradiated Fe9Cr showing helical dislocations in the damaged region and straight dislocations in the unirradiated region.

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Our analysis suggests that a bias of interstitial defects was the cause of the helical form. Dislocation loops were counted and sized using micrographs from several g-vector conditions with varying visible proportions of loops with Burgers vectors of <100> and 1/2<111>. Loop counts were then derived based on statistical analysis. The work on the ion irradiated samples is ongoing, so the number density of dislocation loops visible in a 112-like condition (with one variant of the <111> loops absent) is shown in Figure 4. This analysis shows that far more Figure 4. The number density An interesting observation is that the defects are present in the charged- of dislocation loops visible in dislocations decorated with defects a 112-like condition (with one particle irradiated alloys than the variant of the <111> loops are helical. Ion irradiation has shown neutron irradiated alloy. The cause of absent) is shown here. that the helical shape of the disloca- this difference is likely the dose-rate tion was initially straight and mainly effect because neutron irradiated screw in character (Figure 3). Screw alloys were damaged at a rate that was dislocations can experience a climb ~100 times slower than the charged in response to the absorption of particle irradiated alloys. For a high point defects (interstitial or vacancy), dose rate, cascade-damaged regions which results in the dislocation may be subject to multiple cascades taking a helical shape as it gains in a short space of time, which can edge character, with a Burgers vector inhibit defects from migrating or pointing along the axis of the helix. annihilating. This favours dislocation-

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loop nucleation and may explain the protons will create a larger number of larger number of visible defects in the surviving point defects for the same proton and ion irradiated cases. This dpa dose as ions and neutrons. will also favor a homogeneous spatial Future Activities distribution of dislocation loops. Our future activities include comple- The proton irradiated Fe9Cr alloy tion of the analysis for the Fe6Cr and contains ~2.5 times as many loops improvements to the analysis of the as the equivalent ion irradiated alloy, Fe9Cr. We intend to find the nature despite having been irradiated at the of the loops decorating the helices in same dose rate. This result could be both neutron irradiated alloys and for due to differences in the primary the ion and proton irradiated alloys, knock-on atom (PKA) spectrum of too. Chemical mapping via electron the protons and ions (and neutrons). energy loss spectroscopy is also being Proton irradiation favors lower PKA planned to study chromium precipita- energies; hence, the collision cascades tion (if any). will be small compared to those Publications produced by heavy ions or neutrons. None at present, but we expect the Small cascades result in a greater main results to be published in 2018. proportion of surviving point defects than large cascades, which means that

Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators University of Oxford Jack Haley (co principal investigator), Steve Roberts (principal investigator) University of California, G. Robert Odette (collaborator) Santa Barbara

155 Nuclear Science User Facilities

Removing a fuel element during a routine refueling operation, High Flux Isotope Reactor (HFIR), 156 ORNL (Courtesty of ORNL) 2017 | ANNUAL REPORT

NSUF LIST OF ACRONYMS

ACRR...... Annular Core Research Reactor

AIME...... The American Institute of Mining, Metallurgical, and Petroleum Engineers

AM...... additive manufacturing

AMS...... accelerator mass spectrometry

ANL...... Argonne National Laboratory

ANS...... American Nuclear Society

APS...... Advanced Photon Source

APT...... Atom Probe Tomography

ARRM...... Advanced Radiation Resistant Materials

ATR...... Advanced Test Reactor

BNL...... Brookhaven National Laboratory

BR2...... Belgian Reactor 2

BR3...... Belgian Reactor 3

CAES...... Center for Advanced Energy Studies

CASS...... cast austenitic stainless steel

CCFE...... Culham Centre for Fusion Energy

CDRW...... capacitator-discharge resistance welding

CINR...... Consolidated Innovative Nuclear Research

CNNC...... China National Nuclear Corporation

CNWG...... Civil Nuclear Energy Research and Development Working Group

CoMET...... Combined Materials Experiment Toolkit

CP Ti...... commercially pure titanium

DMLS...... direct metal laser sintering

157 Nuclear Science User Facilities

DOE...... U.S. Department of Energy

DOE-ID...... U.S. Department of Energy Idaho Operations Office

DOE-NE...... Department of Energy Office of Nuclear Energy

EBSD...... electron backscatter diffraction

EDX...... Energy-dispersive X-ray spectroscopy

EIS...... electrochemical impedance spectroscopy

EML...... Electron Microscopy Laboratory

EPMA...... electron probe microscope

EPRI...... Electric Power Research Institute

ETR...... Engineering Test Reactor

EXAFS...... X-ray absorption fine structure

FaMUS...... Fuels and Materials Understanding Scale

FASB...... Fuels and Applied Science Building

FCF...... Fuel Conditioning Facility

FEM...... finite element method

FIB...... Focused Ion Beam

FM...... ferritic-martensitic

FOA...... Funding Opportunity Announcement

FRIB...... Facility for Rare Isotope Beams

FY...... fiscal year

GAIN...... Gateway for Accelerated Innovation in Nuclear

GB...... grain boundary

GIF...... Gamma Irradiation Facility

HDR...... high dose rate

HFEF...... Hot Fuel Examination Facility

HFIR...... High Flux Isotope Reactor

HIP ...... hot isostatic pressing

HIPPO...... High-Pressure-Preferred Orientation

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HPC...... High Performance Computing

I3TEM...... In Situ Ion Irradiation Transmission Electron Microscope

IASCC...... irradiation assisted stress corrosion cracking

IMCL...... Irradiated Materials Characterization Laboratory

INL...... Idaho National Laboratory

ISNAP...... Institute for Structure and Nuclear Astrophysics

IVEM...... Intermediate Voltage Electron Microscope

IYMC...... International Youth Nuclear Congress

JAEA...... Japanese Atomic Energy Agency

JANNuS...... Joint Accelerators for Nanosciences and Nuclear Simulation

LAMDA...... Low Activation Materials Development and Analysis

LANL...... Los Alamos National Laboratory

LANS...... Los Alamos Neutron Science Center

LDR...... low dose rate

LEAP...... Local Electrode Atom Probe

LHMA...... Laboratory for High and Medium Activity

LOI...... Letter of Intent

LWR...... light water reactor

LWRS...... Light Water Reactor Sustainability

MaCS...... Microscopy and Characterization Suite

MFC...... Materials and Fuels Complex

MIBL...... Michigan Ion Beam Laboratory

MIT...... Massachusetts Institute of Technology

MOU...... Memorandum of Understanding

MOX...... mixed oxide

MRCAT...... Materials Research Collaborative Access Team

MSI...... Minority-Serving Institutions

MSTL...... Materials Science and Technology Laboratory

159 Nuclear Science User Facilities

MSU...... Michigan State University

MTR...... Materials Testing Reactor

NADM...... Nuclear Academics Discussion Meeting

NASA...... National Aeronautics and Space Administration

NEID...... Nuclear Energy Infrastructure Database

NFMC...... Nuclear Fuels and Materials Characterization Facility

NFML...... Nuclear Fuels and Materials Library

NPIC...... Nuclear Power Institute of China

NRC...... U.S. Nuclear Regulatory Commission

NRL...... Nuclear Reactor Laboratory

NSCL...... National Superconducting Cyclotron Laboratory

NSLS...... National Synchrotron Light Source

NSUF...... Nuclear Science User Facilities

NuMat...... Nuclear Materials Conference

ODS...... Oxide-Dispersion-Strengthened

ORNL...... Oak Ridge National Laboratory

OSU ...... The Ohio State University

OSURR...... The Ohio State University Research Reactor

PDC...... polymer-derived ceramics

PFC...... planning and financial control specialist

PIE...... post-irradiation examination

PKA...... primary knock-on atom

PM...... powder metallurgy

PNNL...... Pacific Northwest National Laboratory

PPMS...... Physical Properties Measurement System

RaDIATE...... Radiation Damage In Accelerator Target Environments

RAFM...... reduced activation ferritic-martensitic

RIS...... radiation induced segregation

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RPV...... Reactor Pressure Vessel

RT ...... room temperature

RTE...... Rapid Turnaround Experiment

SCC...... stress corrosion cracking

SCK•CEN...... Studiecentrum voor Kernenergie • Centre d’Etude de l’Energie Nucleaire / Belgian Nuclear Research Centre

SEM...... scanning electron microscopy

SIBL...... Sandia National Laboratories Ion Beam Laboratory

SMARTS...... Spectrometer for Materials Research at Temperature and Stress

SNICS...... Source of Negative Ions by Cesium Sputtering

STIP...... Spallation Target Irradiation Program

SULI...... Summer Undergraduate Laboratory Internship

TEM...... transmission electron microscopy

TMS...... The Minerals, Metals and Materials Society

TREAT...... Transient Reactor Test Facility

TRTR...... Test, Research, and Training Reactors

TTAF...... Test Train Assembly Facility

UCB ...... University of California, Berkeley

UCBNE...... University of California, Berkeley Nuclear Engineering

UCSB...... University of California, Santa Barbara

WBDF...... weak-beam dark field

XRD...... x-ray diffraction

XRF...... x-ray fluorescence

161 Nuclear Science User Facilities

NSUF INDEX

NSUF & Partner Institutions: Idaho National Laboratory: Los Alamos National Laboratory: 9, 19, Facilities & Capabilities Advanced Test Reactor (ATR), 8, 9, 28, 54, 36, 39, 55, 56, 73, 75, 81, 86, 87, 90, 91, Argonne National Laboratory: 18, 68, 64, 68, 70, 73, 76, 77, 78, 83, 84, 89, 90, 93, 161, 162 69, 70, 72, 73, 75, 76, 77, 78, 80, 86, 87, 91, 92, 101, 105, 112, 113, 115, 151, Los Alamos National Laboratory: 115, 122, 125, 126, 130, 131, 136, 138, 157, 160, Cover Photo Chemical and Metallurgical Research Facility 141, 161, 162 Idaho National Laboratory: (Wing 9), 93 Argonne National Laboratory: Analytical Laboratory, 160 Los Alamos National Laboratory: Intermediate Voltage Electron Microscopy Idaho National Laboratory: Lujan Center at Los Alamos Neutron Science (IVEM)-Tandem Facility, 68, 69, 70, 72, 73, Electron Microscopy Laboratory (EML), 41, Center (LANS), 55 75, 76, 77, 78, 80, 122, 125, 130, 136, 137, 42,119, 157, 160 138, 141 Los Alamos National Laboratory: Idaho National Laboratory: Fuels and Plutonium Surface Science Laboratory, 56 Brookhaven National Laboratory: 9, 18, Applied Sciences Building (FASB), 12, 48, 158 24, 54, 86 Massachusetts Institute of Technology: Idaho National Laboratory: 16, 33, 73, 76, 84, 86, 87, 132, 135, 158, 160 Brookhaven National Laboratory: Gamma Irradiation Test Loop, 12 National Synchrotron Light Source II, 24, 54 Massachusetts Institute of Technology: Idaho National Laboratory: Nuclear Reactor Laboratory, 23, 56 Center for Advanced Energy Studies Hot Fuel Examination Facility (HFEF), 2, (CAES): 9, 15, 16, 27, 32, 33, 63, 68, 69, North Carolina State University: 16, 33, 43, 158 70, 72, 74, 75, 76, 77, 78, 80, 86, 87, 103, 69, 76, 84, 86, 87, 109, 111, 160 Idaho National Laboratory: 105, 117, 119, 129, 130, 131, 141, 151, North Carolina State University: Irradiated Materials Characterization Laboratory 152, 153, 155, 157, 160 PULSTAR Reactor Facility, 33, 34, 111 (IMCL) Facility, 78, 94, 95, 96, 99 Center for Advanced Energy Studies Oak Ridge National Laboratory: 13, 17, Illinois Institute of Technology: 16, 86, (CAES):Microscopy and Characterization Suite 31, 68, 69, 70, 72, 73, 75, 76, 77, 78, 82, 87, 115, 160 (MaCS), 63, 68, 72, 75, 76, 77, 78, 80, 103, 83, 86, 87, 94, 98, 99, 123, 124, 133, 135, 105, 119, 129, 131, 141, 155, 158, 160 Illinois Institute of Technology: 142, 144, 149, 156, 158, 160, 161 Materials Research Collaborative Access Team Idaho National Laboratory: 2, 3, 4, 5, Oak Ridge National Laboratory: Gamma (MRCAT), 113, 114, 115, 158 8, 9, 10, 12, 13, 14, 16, 18, 21, 22, 26, 28, Irradiation Facility, 57 29, 30, 35, 39, 40, 41, 42, 43, 44, 45, 46, Lawrence Livermore National Oak Ridge National Laboratory: 48, 49, 51, 52, 53, 57, 60, 63, 64, 68, 69, Laboratory: 9, 19, 55, 86 70, 71, 72, 73, 75, 77, 78, 79, 80, 83, 86, High Flux Isotope Reactor (HFIR), 31, 83, 87, 89, 101, 103, 105, 112, 113, 115, 116, Lawrence Livermore National 133, 156, 160 Laboratory: Center for Accelerator Mass 117, 119, 136, 137, 141, 151, 153, 158, Oak Ridge National Laboratory: Spectrometry, 55 160, 161 162 Low Activation Materials Design and Analysis Laboratory (LAMDA), 68, 69, 70, 72, 73, 75, 76, 77, 94, 99, 123, 124, 133, 135, 160

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Attendees at the NSUF-GAIN Thermal Hydraulics Workshop, INL Meeting Center, INL (Chris Morgan, INL)

The Ohio State University: 9, 19, 23, 56, Sandia National Laboratories: In Situ University of Michigan: 16, 69, 70, 72, 86, 87, 163 Ion Irradiation Transmission Electron Microscope 77, 86, 87, 94, 99, 104, 160 (13TEM) Facility, 57, back cover Pacific Northwest National Laboratory: University of Michigan: 17, 20, 75, 80, 83, 84, 87,159, 160 Texas A&M University: 9, 19, 58, 77, Michigan Ion Beam Laboratory, 77, 94, 160 86, 87 Pacific Northwest National Laboratory: University of Nevada, Las Vegas: 17, 86 Materials Science & Technology Laboratory Texas A&M University: University of Wisconsin: 17, 70, 72, 73, (MSTL), 20 Accelerator Laboratory 58 76, 77, 80, 86, 87, 160, 162 Pacific Northwest National Laboratory: University of California, Berkeley: 17, University of Wisconsin: Characterization Radiochemistry Processing Laboratory, 75, 80 36, 37, 38, 68, 86, 87, 93, 148, 149,160 Laboratory for Irradiated Materials, 70, 77 Purdue University: 17, 27, 70, 72, 73, University of California, Berkeley: University of Wisconsin: Tandem 86, 87, 137, 160 Nuclear Materials Laboratory, 93, 148, 149, Accelerator Ion Beam, 70, 77, 160 160, Purdue University: Interaction of Materials Westinghouse: 6, 18, 60, 61, 67, 84, 86, with Particles and Components Testing University of Florida: 9, 19, 40, 41, 42, 87 160 (IMPACT) experimental facility, 62 43, 58, 69, 70, 75, 76, 78, 80, 86, 87, 119, 130, 131, 161, 162 Westinghouse: Churchill Site, 6, 18, 60, Sandia National Laboratories: 9, 18, 57, 61, 67, 84, 86, 87 160 75, 85, 86, 87, back cover University of Florida: Nuclear Fuels and Materials Characterization Facility, 43, 58 Sandia National Laboratories: Gamma Irradiation Facility, 57

163 Nuclear Science User Facilities

Collaborators Katoh, Yutai Post Guillen, Donna Aitkaliyeva, Assel Oak Ridge National Laboratory 75, 133, Idaho National Laboratory 112, 113, 115 University of Florida 40, 119, 161 142,149 Roberts, Professor Steve Amroussia, Aida Kirk, Marquis A. University of Oxford 100, 103, 105, 150 Michigan State University 72, 125 Argonne National Laboratory 122, 141 Roberts, Steve Bachhav, Mukesh Koyanagi, Takaaki University of California, Santa Barbara 155 Idaho National Laboratory 77, 78, 104, 119 Oak Ridge National Laboratory 133, 149 Saleh, Tarik A. Boehlert, Carl Krumwiede, David Los Alamos National Laboratory 90, 93 Michigan State University 120, 125 University of California, Berkeley 91, 93 Snead, Lance Chen, Wei-Ying Leonard, Keith Massachusetts Institute of Technology 132, Argonne National Laboratory 80, 126, Oak Ridge National Laboratory 99 133, 135 129, 131 Li, Meimei Song, Miao Chen, Yiren Argonne National Laboratory IVEM – Tandem University of Michigan 94, 99 Argonne National Laboratory 68, 131, 161 Facility 122, 125, 131 Taylor, Joanna Cheng, Steven Maloy, Stuart A. Idaho National Laboratory 105, 162 Rutgers University 115 Los Alamos National Laboratory 93, 161 Wang, Mi Gan, Jian Miller, Brandon University of Michigan 99, 139 Idaho National Laboratory 141 Idaho National Laboratory 116, 117, 119 Was, Gary Gragg, David Mittig, Wolfgang University of Michigan 99 University of California, Santa Barbara National Superconducting Cyclotron Wells, Peter 103, 105 Laboratory (NSCL), Facility for Rare Isotope University of California, Santa Barbara 70, Beams (FRIB) 125 Haley, Jack 103, 105, 162 University of California, Santa Barbara Odette, G. Robert - Odette, G. R. Xu, Cheryl 153, 155 University of California, Santa Barbara 93, Florida State University 76, 106, 111, 131 103, 105, 151, 155, 161 He, Lingfeng Yang, Yong Idaho National Laboratory 73, 136, 141 Pathania, Raj University of Florida 70, 80, 131, 149. 162 Electric Power Research Institute 99 Hewitt, Luke University of Oxford 101, 102, 103, 105 Pellemoine, Frederique National Superconducting Cyclotron Hosemann, Peter Laboratory (NSCL), Facility for Rare Isotope University of California, Berkeley 36, 37, 38, Beams (FRIB) 125 39, 93, 149, 161 Porter, Douglas Kabel, Joey Idaho National Laboratory 115 University of California, Berkeley 145, 148, 149

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Cherenkov radiation, The Ohio State University Research Reactor (OSURR), The Ohio State University (Courtesy of The Ohio State University) 165 Researchers working in the In situ Ion Irradiation Transmission Electron Microscope (I3TEM) Facility, Sandia Ion Beam Laboratory, Sandia National Laboratories (Courtesy of Sandia National Laboratories)

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