2016 I ANNUAL REPORT Nuclear Science User Facilities
/"'7 Nuclear Science ,'-- @ ilJU-r User Facll1tles J Nuclear Science User Facilities
Analytical Laboratory, Materials & Fuels Complex (MFC), Idaho National Laboratory (INL)
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-17-43047 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, 2015, through September 30, 2016) 2 2016 | ANNUAL REPORT
OUR NSUF TEAM J. Rory Kennedy Director (208) 526-5522 [email protected]
Dan Ogden Jeff Benson Deputy Director Program Administrator (208) 526-4400 (208) 526-3841 [email protected] [email protected]
Brenden Heidrich Collin Knight Capabilities Scientist Post-irradiation (208) 533-8210 Examination Coordinator [email protected] (208) 533-7707 [email protected]
John Jackson Keith Jewell Industry Program Lead Research Scientist (208) 526-0293 (208) 526-3944 [email protected] [email protected]
Kelly Cunningham Jonathan Kirkham Nuclear Fuels and Scientific Support Professional Materials Library Coordinator (208) 533-8188 (208) 526-2369 [email protected] [email protected]
John Coody Lindy Bean Project Scheduler Financial Controls Specialist (208) 526-2964 (208) 526-4662 [email protected] [email protected]
Laura Scheele Renae Soelberg Communications Liaison Administrative Assistant (208) 526-0442 (208) 526-6918 [email protected] [email protected] Nuclear Science User Facilities
4 Neutron Radiography Reactor (NRAD), MFC, INL 2016 | ANNUAL REPORT
TABLE OF CONTENTS
Nuclear Science User Facilities • From the NSUF Director ...... 7 • Q&A with Tom Miller ...... 11 • Focus on New Staff ...... 14 • Researcher Profiles ...... 22
NSUF Overview • Program Overview ...... 30 • A Tremendous Success: CINR FOA ...... 32 • RTE/Beamline Demand Increases ...... 34 • New NSUF Partner Facility: IVEM-Tandem ...... 37 • Nuclear Fuels and Materials Online Library ...... 38 • NSUF at Work: Ion Beam Capabilities ...... 40
Distributive Partnerships Map • Distributed Partnerships ...... 44
NSUF Projects • Awarded Projects ...... 47
Resources • Acronyms ...... 95 • Index ...... 98 Nuclear Science User Facilities
X-Ray Diffraction, Microscopy and Characterization Suite (MaCS), 6 Center for Advanced Energy Studies (CAES) 2016 | ANNUAL REPORT
FROM THE NSUF DIRECTOR
J. Rory Kennedy Director (208) 526-5522 [email protected]
he Nuclear Science User The NSUF team has also grown to other related information from both Facilities (NSUF) will celebrate support a research and development U.S. and international institutions. Tour 10th anniversary in 2017. ecosystem to better enable high-impact Created in fiscal year (FY) 2015, the Since it was originally founded as nuclear energy research. We welcomed NEID is designed to be a tool for the Advanced Test Reactor National three new team members in 2016 who researchers and developers across federal Scientific User Facility (ATR-NSUF), are profiled in this report: government agencies, the national the NSUF has grown into a truly laboratory system, industry, universities, • Kelly Cunningham, Nuclear Fuels & national – and international – and international organizations. Materials Library Coordinator, organization. Speaking of the ATR, this In 2016, the NSUF made the NEID national research treasure will also be • Jonathan Kirkham, Scientific Support database available to the newly celebrating its 50th anniversary in July Professional, and established Gateway for Accelerated 2017. Established in 2007, the NSUF • John Coody, Project Scheduler. Innovation in Nuclear (GAIN) initia- has focused on the goal of serving as With our added team members, we tive to facilitate GAIN industry users’ a scientific and technical foundation continued to enhance two important identification of capabilities that can for the U.S. Department of Energy’s NSUF resources: the Nuclear Fuels advance their technologies. The NSUF Office of Nuclear Energy (DOE-NE) as and Materials Library (NFML) and the is pleased to engage with the GAIN it advances nuclear power to meet our Nuclear Energy Infrastructure Database initiative in its mission to provide nation’s energy, environmental, and (NEID). Kelly Cunningham brought industry innovators the technical and national security needs. the NFML online as a web-based, regulatory support they need to move The NSUF’s shared history with ATR searchable database of legacy irradiated new or advanced nuclear technology brings into focus the tremendous nuclear fuels and materials available to concepts and designs toward commer- asset that ATR has provided to nuclear the nuclear community for advanced cialization. The combined resources energy researchers and innovators. scientific studies. Jonathan Kirkham, offered through the NSUF and the The NSUF has completed 13 ATR working with NSUF Capabilities Coor- GAIN initiative provide an unprec- irradiations and currently has five ATR dinator Brenden Heidrich, continued edented diversity of nuclear energy projects underway. NSUF researchers to build out the NEID database. In researchers and innovators access to have published over 28 refereed journal September 2016, it contained data from world-class capabilities, infrastructure, papers to date based on research up to 127 institutions supporting about and expertise in all aspects of nuclear utilizing the ATR. 465 facilities that house close to 1,000 energy technologies. instruments and equipment, including research and test reactors, conventional 2016 was a banner year for the and advanced instrumentation as well as NSUF in both the number of proposals received and the number and value of projects awarded. This
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is a clear indication of the worth NSUF organized a session at the ANS the Transient Reactor Test (TREAT) that the nuclear energy research winter meeting and, together with Facility, and High Temperature Test community finds in the NSUF, and the NSUF Users Organization, will Laboratory (HTTL) in the United bringing on John Coody has allowed continue organizing NSUF conference States. Other NSUF facilities may be the NSUF to continue to manage sessions in the future to showcase the brought in at a later time. We expect this increasing volume of projects science we are producing. a Memorandum of Understanding to effectively. In FY 2016, the NSUF be signed between DOE-NE and the Our researchers are achieving scientific awarded 39 projects from a pool of Belgian SCK-CEN in the early part of prominence by publishing and docu- 75 applications from 24 institutions FY 2017. menting research results through peer- during the thrice-yearly Rapid reviewed journals and presentations at Looking further ahead in 2017, we are Turnaround Experiments solicitations, conferences. We recorded the highest working to provide our users access a 30 percent increase in awarded number of journal publications in to additional capabilities, such as the proposals and a 60 percent increase NSUF history in 2016 with 55, which National Synchrotron Light Source in proposals received over FY 2015 beat the previous high of 33 in 2015. II (NSLS-II) at Brookhaven National respectively. The annual Consolidated Due to the nature of NSUF related Laboratory. Several other institutions Innovative Nuclear Research (CINR) research, which can require longer have expressed interest in joining the Funding Opportunity Announcement time duration to yield results from NSUF Partner Facilities consortium and (FOA) drew 67 pre-applications (a experiments that tend to involve greater we will evaluate their applications in 116 percent increase) with final expense and require access to special- 2017. We will build on the produc- submissions of 32 full applications ized and unique facilities, we expect tive outcomes from the FY 2016 Ion (an 88 percent increase) resulting in our publication record to continue to Beam Workshop by bringing together 12 awards (a 160 percent increase) increase as we reap the benefits from a committee to develop an Ion Beam totaling about $10 million in support earlier irradiation tests. Since the NSUF Utilization Roadmap. We look forward (up from $4.2 million in FY 2015). works to reduce barriers to research, to hosting a Thermal Hydraulics To expand user awareness of our capa- the steady growth in publications is Workshop to identify potential research bilities, the NSUF maintains an active testimony to DOE-NE’s commitment to opportunities as part of an expanded presence in research-related circles. We advancing nuclear energy. NSUF scope. Finally, we will hold exhibited in FY 2016 at the American our inaugural NSUF Partner Facilities FY 2016 saw the NSUF expand its Nuclear Society (ANS) winter meeting, Working Group meeting in an effort to associations in the international the Electric Power Research Institute better engage our Partner Facilities in arena. We continued our interactions (EPRI) International Light Water the activities of the NSUF. with the UK’s National Nuclear User Reactor Materials Reliability Confer- Facility and finalized discussions with Please take a few moments to learn ence, the Materials Research Society the SCK-CEN Belgian Nuclear Research more about all the important nuclear (MRS) fall meeting, The Minerals, Centre on a pilot project involving research facilitated by NSUF at Idaho Metals and Materials Society (TMS) irradiations in the ATR and Belgium National Laboratory and our diverse spring meeting, and the Nuclear Reactor-2 (BR-2). This will be mix of affiliated partner institutions Materials Conference (NuMat). Our followed by post-irradiation examina- across the United States I thank the impact becomes greater as tradition- tion (PIE) activities at the Laboratory NSUF partners and users for their hard ally non-nuclear focused researchers for High and Medium Activity at the work to make the NSUF a successful understand the opportunities posed Belgian Nuclear Research Centre and strategic research organization. in working in the nuclear field and at Idaho National Laboratory (INL) how they can benefit from capabilities Materials and Fuels Complex (MFC), offered by the NSUF. In addition, the
J. Rory Kennedy
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Focused Ion Beam Confinement Box, Irradiated Materials Characterization Laboratory (IMCL), MFC, INL9 Nuclear Science User Facilities
10Local Electrode Atom Probe (LEAP), MaCs, CAES 2016 | ANNUAL REPORT
Q&A WITH TOM MILLER
Director Office of Accelerated Innovation in Nuclear Energy U.S. Department of Energy
Q: Can you tell us more about what you do at Q: What other areas have you worked with Q: What got you interested in nuclear energy? the Department of Energy Headquarters (U.S. while at DOE? A: During my sophomore year in DOE-HQ)? A: I have worked for the Office of college, I did a paper on the NS A: Currently, my role within the Nuclear Energy throughout my tenure Savannah, the first commercial nuclear Office of Nuclear Energy is to with DOE in a variety of programmatic powered ship. As a maritime student, direct and manage those research, roles supporting the deployment I was intrigued with the commercial development, and infrastructure of new reactor technology. Most applications of nuclear energy. programs that support the accelerated recently I served as the director for the Q: What brought you to NSUF oversight? development of innovative nuclear Light Water Technology Office with technology. The Nuclear Science User responsibilities for the Small Modular A: Actually, it was the result of a Facilities (NSUF) is one of the key Reactor Licensing Technical Support job offer I couldn’t refuse as part of programs within my responsibilities. and Light Water Reactor Sustainability a reorganization. programs. Prior to that, I was Q: What are some of your other responsibilities? Q: What do you like to do outside of the office responsible for the development and (hobbies, volunteer activities, interests)? A: Other key program responsibilities implementation of the Nuclear Power include the Nuclear Energy Enabling 2010 program, which supported the A: My wife (mostly) and I operate a Technology (NEET) program technology and licensing of the first horse farm. We board and take care of sponsoring research in advanced new nuclear plants to be built in the other people and our own horses. It is modeling and simulation, advanced United States in over 30 years. a lot of work, but we enjoy it. My wife sensors and instrumentation, and is an avid rider and fox hunter. Q: What did you do prior to joining DOE-HQ? advanced methods for manufacturing. Q: The NSUF is celebrating its 10th anniversary In addition, I have responsibility for A: I worked in the commercial in 2017. What do you see as the NSUF’s the university programs involving nuclear industry for 26 years prior to greatest accomplishments? scholarships, fellowships, university joining the DOE in a variety of roles reactor fuel, and the university research and positions. A: Establishing the Advanced Test and development program. Reactor – National Scientific User Q: What’s your educational background? Facility, as it was originally known, Q: How long have you been with DOE? A: Bachelor’s degree in Nuclear Science was a significant success, but A: I joined the U.S. Department of from the State University of New York recognizing that the needs of the Energy in 1999. Maritime College nuclear energy community extended beyond the original irradiation and post irradiation examination capabilities, and moving into the
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NSUF consortium that exists today is people operating these facilities and how it benefits DOE-NE, we’re able to one of its greatest achievements. The equipment. Being the link between all allocate more funding to more awards range of facility representation and of those components will truly help through the use of this database. That is capabilities in the NSUF consortium the understanding and advancement of a great advantage for everyone. from universities, national laboratories, nuclear energy. Q: How is the NSUF viewed by DOE-NE? and even industry is very unique and Q: What are challenges facing the NSUF? quite impressive, encompassing a A: DOE-NE relies on the NSUF to broad range of irradiated materials A: The current challenge, and I make those connections to physical science. In late 2016, the NSUF think this is an agreement across equipment, samples, researchers, established an international partnership the community, is the availability of knowledge, data, and other aspects agreement with the Belgium research neutrons. The NSUF originally began within the nuclear energy research reactor to further expand its research as a way to provide access to the framework. Because of this, we look infrastructure capabilities. And new Advanced Test Reactor, but space in the at the NSUF as the vital partner capabilities and facilities are being reactor has become limited in recent to the Gateway for Accelerated examined yearly, all in an effort to years. Limited space at the nation’s Innovation in Nuclear (GAIN) continuously support the nuclear top materials test reactor is, of course, initiative to help the advancement stakeholder community and provide reflective of the revitalization of nuclear of nuclear energy. The NSUF the necessary access to support the energy, but it has also made the NSUF provides that lower level Technology advancement of nuclear energy. look at alternatives for meeting the Readiness Level (TRL) research that community’s demand. To help offset supports the greater industry. The NSUF also took on the challenge the demand for the ATR, the NSUF to develop and maintain the Nuclear Q: If you look into your crystal ball, what is partnered with a number of test Energy Infrastructure Database, which changes do you see in store for the NSUF over the reactors within the United States and was no small feat, and was able to next ten years? has recently signed a Memorandum release this unique capability in of Understanding with the Belgian A: The NSUF is currently focused on FY 2016. We’ve received feedback Research Reactor in Belgium. irradiated materials characterization, from both users and facilities that the which will certainly provide the Q: The Nuclear Fuels and Materials Library in database does a great job identifying data needed by the advanced reactor FY 2016 evolved from spreadsheet data to an relevant nuclear related infrastructure. community. Moving forward, it online database searchable by researchers. How do Building upon that success, the Nuclear is important to look at what other you foresee the NFML benefiting DOE-NE? Fuels and Materials Library will further research infrastructure is needed by assist researchers by identifying A: I see this capability as one more the stakeholder community, whether available irradiated specimens to component to the NSUF’s access. We this capability is available within the examine at those available facilities. already discussed the NEID and this laboratory and university community, Q: Where do you see the NSUF’s database will further assist the user and whether DOE investment in this best opportunities? community in accessing necessary capability is necessary. The NSUF irradiated materials that have a team has been doing this with a focus A: The NSUF’s best opportunities known pedigree. Those samples come on irradiated materials and now is are the access the program provides from industry, national laboratories, expanding to look at other nuclear for researchers to unique nuclear previously funded NSUF projects, science areas. As we move forward, the irradiation and post-irradiation and samples that have been identified NSUF team will be looking to support examination capabilities – not only by the community for the NSUF to the advancement of nuclear energy to the physical instruments, but the irradiate through a series of Sample across a broad array of R&D areas, such knowledge, data, and expertise of the Library (SAM) experiments. As to as thermal hydraulics and other related advanced reactors areas.
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Analytical Laboratory, MFC, INL 13 Nuclear Science User Facilities
FOCUS ON NEW STAFF
Kelly Cunningham Coordinator for the Nuclear Fuels and Materials Library uclear Science User Facilities Cunningham is used to tackling new (NSUF) researchers access the challenges. Upon earning her degree NNuclear Fuels and Materials in radiographic science, she worked Library to locate irradiated material and for a few years as a radiographic and fuel samples for further experimenta- MRI technologist in health sciences. tion. Kelly Cunningham is charged She joined Battelle Energy Alliance, with keeping the library information LLC in 2004 and initially worked at current, relevant to the NSUF mission, the Materials and Fuels Complex as a and available to researchers. Health Physics Technician. Over time, she worked in a variety of laboratory The Nuclear Fuels and Materials mission areas, including National & Library is owned by the U.S. Depart- Homeland Security, before joining ment of Energy Office of Nuclear the NSUF. Energy (DOE-NE) and curated by the NSUF. The Library is a collection of “The best part of my time with specialized information and nuclear Idaho National Laboratory (INL) has fuel and material specimens from been the people,” Cunningham said. past and ongoing irradiation test “Working with really supportive campaigns, real-world components people on interesting and important retrieved from decommissioned projects keeps me engaged.” power reactors, and donations from The original materials database other sources. contained approximately 3,500 Cunningham’s role when joining specimens, including legacy materials, the NSUF was to transform the volunteered materials, and NSUF information contained in multiple project specimens. Most specimens spreadsheets into an online library had been neutron irradiated; some to provide intuitive access to users. were proton irradiated. The spread- “Taking on a brand new project sheets were eventually consolidated that had the potential to make and migrated into an online database researchers’ lives easier was exciting,” with the help of an NSUF dedicated Cunningham said. “I like being the information management specialist. person who works with specialists to resolve any issues a researcher has when using the library.”
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Transmission Electronic Microscope (TEM), Materials Science & Technology Laboratory, Pacific Northwest National Laboratory (PNNL) - Courtesy of PNNL 15 Nuclear Science User Facilities
Research Sample, Radiochemistry Laboratories, University of Nevada - Las Vegas 16 2016 | ANNUAL REPORT
“The biggest challenge we have is that “The NSUF Nuclear Fuels and the information has been provided by Materials Library will continue to different researchers that don’t use the be a valuable research portal to same names for the same materials,” support scientific outcomes,” said Cunningham explained. “Developing Cunningham. “I enjoy hearing the a consistent nomenclature will Principal Investigators present findings “Developing a consistent streamline searches and continue the based on experiments done evolution of developing the database with Library materials, and I’m into a true Library.” always interested in hearing feedback nomenclature will streamline and suggestions on how to improve The NSUF’s goal is to have the Library the Library.” continue to expand and showcase searches and continue the the available range of samples and Read more about the NSUF Nuclear Fuels and experimental data. This goal means Materials Library on page 38. evolution of developing the that Cunningham will continue to work with national labs, universities, and industry to collect valuable database into a true Library.” materials into a single, public repository that serves the nuclear community and DOE-NE’s mission.
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Jonathan Kirkham Keeper of the Nuclear Energy Infrastructure Database (NEID)
ow the Nuclear Science User a research assistant and consultant in Facilities (NSUF) interacts Boise before joining the NSUF staff in Hwith the United States nuclear October 2015. industry and research community Making the jump from physics to depends to a great extent on the materials science has meant learning information that’s available to them. about procedures and equipment. As the scientific support specialist Making use of the environment at the responsible for the Nuclear Energy Center for Advanced Energy Studies Infrastructure Database (NEID), and its affiliation with four universi- Jonathan Kirkham plays a critical role ties, Kirkham is pursuing a master’s in on the NSUF staff. nuclear engineering. The purpose of the NEID is to provide In 2016, one of his projects was to information on all capabilities and update the NEID’s online presence. In facilities related to nuclear energy, accomplishing this, he has managed to including institutions, facilities, and give it: instrumentation. This gives members of the nuclear research community • A new look, feel, and the means to search for capabilities navigation properties on current or future projects. For the • Editing capabilities for institution U.S. Department of Energy Office of officials and facility owners Nuclear Energy, it provides aid for • New coordinate mapping through infrastructure investment decisions. For Google Maps the NSUF itself, it allows staff members • User profiles interconnected to search for the best and most cost throughout all NSUF databases effective capabilities available. The NEID provides support for the Gap Analysis • User sign-up through the main Report, Nuclear Energy Request for NSUF webpage Information (RFI), and Nuclear Energy • The ability to save a list of facilities Infrastructure Funding Opportunity or instruments for quicker access Announcements (FOAs). The NEID webpage can be accessed For Kirkham, the challenge is keeping through NSUF’s main webpage or at the information complete and up to nsuf-infrastructure.inl.gov. date, scouring reference sources for As of September 2016, NEID had data little known or overlooked resources from 127 institutions, 465 facilities, and (i.e., “Trying to find a lot of stuff that’s 963 instruments. The majority of insti- not published in anything.”). An Idaho tutional data – 79.5 percent — came Falls native who graduated from the from universities (49), government University of Idaho with a bachelor’s (30) and industry (22) in the United in physics, Kirkham was working as States. The remainder came from corresponding international sources.
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Irradiation Assisted Stress Corrosion Cracking Facility, Energy Innovation Laboratory (EIL), INL 19 Nuclear Science User Facilities
Irradiated Materials Characterization 20 Laboratory (IMCL), MFC, INL 2016 | ANNUAL REPORT
John Coody NSUF scheduler at home in Project Controls
s scheduler for the Nuclear Coody said his experience at D.C. Cook Science User Facilities (NSUF), gave him valuable insight into one of AJohn Coody is used to keeping the NSUF’s key missions, the life cycle a lot of balls in the air. extension of nuclear power plants. “It’s important now because all the His job involves working with plants are aging,” he said. “The newest researchers and experiment nuclear plants were built in the late managers, looking at a scoping ‘70s or early ‘80s and back then they statement, and figuring out when were only licensed for 30 years.” (D.C. to schedule design, fabrication, Cook’s two units, which went online in assembly, irradiation, post- 1975 and 1978, have been relicensed irradiation examination, and by the Nuclear Regulatory Commission disposition of materials. But Project through 2034 and 2037.) Control is something that comes naturally, perhaps even by birth. Coody said what he likes best about His father, also John Coody, was a working for the NSUF is the variety. project controller for EG&G Idaho Since coming, he has worked on and Lockheed Martin Idaho. projects with GE Hitachi, Idaho State University, Boise State University, and When Coody came to work for the Colorado School of Mines. With the NSUF in May 2016, it was after 20 number of Consolidated Innovative years of working project controls for Nuclear Research (CINR) projects U.S. Department of Energy (DOE) and Rapid Turnaround Experiments contractors at Los Alamos National (RTEs) rising sharply (from 2015 to Laboratory, Hanford, Savannah River, 2016, CINR full project applications and Idaho National Engineering went from 17 to 32 and RTE project and Environmental Laboratory. In applications rose from 47 to 75), the private sector, he worked for the pace of work shows no sign of Motorola and at the Donald C. slowing down. Cook Nuclear Generating Station in southwest Michigan. “We’re doing something different all the time,” Coody said.
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RESEARCHER PROFILES
Matt Swenson The NSUF enables researcher journey from Boise State University student to University of Idaho Assistant Professor
or a textbook case of how the Swenson joined Wharry’s group at Nuclear Science User Facilities BSU in June 2013. One of the first F(NSUF) is supposed to work, things she had him do was attend one might not need look further than the NSUF Users Week in Idaho Falls. Matthew Swenson, who defended his “I think, in hindsight, it was a really doctoral dissertation in May 2017 and good thing for him,” she said. “He is headed to the University of Idaho in was exposed to all the research that the fall to be an assistant professor in was going on in the nuclear materials mechanical engineering. world and got to meet other students and learn what they were doing.” “The NSUF has been the complete enabler of all my research,” he said. Not only did it give him a full picture of the research, “It gave me an After graduating from Oregon State orientation on how the process works, University, Swenson spent 14 years how proposals were to be written,” in the heavy equipment industry Swenson said. as an engineering manager and platform leader. “All along I knew I His research has focused on radiation was interested in graduate studies and resistance of iron based steel alloys obtaining an advanced degree,” he said. containing nanoparticles, used as cladding and structural components When he enrolled in Boise State in nuclear reactors, optimizing the University’s (BSU) materials science microstructures to improve their and engineering program in 2013, he durability under irradiation. More found a mentor in Dr. Janelle Wharry, particularly, he has been developing lab whose focus was on irradiation experiments that use charged particles experiments and introduced him to to emulate what is happening in nuclear nuclear materials. reactors. Experiments with charged BSU is a member of the consortium particles can be done in days rather that forms the Center for Advanced than months, and the materials are not Energy Studies, where the NSUF has radioactive at the end of the experiment. its offices. Over three years, Swenson estimated he made the 570 mile round-trip between Boise and Idaho Falls between 25 and 30 times.
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Matt Swenson, MaCS, CAES23 Nuclear Science User Facilities
24 Atom Probe Tomography, MaCS, CAES 2016 | ANNUAL REPORT
“We’re hoping to have a calculation His involvement in the NSUF has model that can be used as a predictive led to a seat as the student member tool for folks developing alloy on the NSUF Users Organization’s materials for reactors,” he said. Executive Committee, which serves as an advocacy group for the NSUF’s For the necessary comparisons, experimental activities and provides Swenson has used data collected on “It works really well to make a communication channel among materials exposed to radiation in users of the NSUF. “The networking Idaho National Laboratory’s (INL) opportunity really makes a big Advanced Test Reactor, the NSUF’s a sample at CAES, do difference,” he said. original asset and still one of its most important. Wharry, now at Purdue University, analysis onsite at CAES with views the NSUF as essential to Swenson was awarded his first project, Swenson’s success. “I don’t think I can entitled “Understanding the Effects of give enough credit to how important the tools at MaCS, then take Irradiation Dose Rate and Particle Type it was as a resource to him,” she said. in Ferritic/Martensitic Alloys” in 2015. “The rapid turnaround projects gave The award provided him with access to all the data home. Without him a lot of experience to help him materials characterization equipment become proficient in microscopy.” at the NSUF, where he compared the the resources at CAES, I effects of charged particle irradiation They also provided a learning curve to neutron irradiation on the for proposal writing – a skill all microstructural evolution of advanced graduate students need to learn. probably would have picked F/M alloys HT9 and HCM12A. “Writing his own proposals, I think that was a really big step for him,” He made use of the Microscopy and a different school than Boise she said. Characterization Suite (MaCS) at the Center for Advanced Energy Studies Wharry said the NSUF is a resource State University.” (CAES), with instruments such as the she plans to continue to use with her focused ion beam (FIB), transmission students. One of her Purdue students, electron microscope (TEM), and Keyou Mao, had plans to spend more Localized Electron Atom Probe (LEAP). than a month at CAES in summer “It works really well to make a sample 2017. “It’s an incredible resource,” at CAES, do analysis onsite at CAES she said. “I’ve seen this model that has with the tools at MaCS, then take all worked really well for Matt and me.” the data home,” he said. “Without the resources at CAES, I probably would have picked a different school than Boise State University.”
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Yong Yang Users Organization: Building continuity to secure the NSUF’s future
n the evolution of any the future,” he said. His research organization, institutional memory focus shifted to radiation damage Iand continuity are key to long- occurring in light water reactor core term success. As the Nuclear Science structural components. User Facilities (NSUF) approaches its Yang was one of the 68 people – tenth anniversary, some of the people students, university faculty, and who were “present at the creation” in industry representatives – to attend support roles have become the leaders. the first weeklong ATR NSUF summer Now an associate professor of nuclear sessions, which eventually became engineering at the University of Florida, known as Users Week. It featured Dr. Yong Yang was a postdoctoral fellow presentations by 19 technical experts of Dr. Todd Allen at the University and covered topics such as irradiation of Wisconsin in 2008 when he damage mechanisms, degradation participated in the Advanced Test Reactor of reactor materials, light water (ATR) NSUF pilot experiment. reactor and gas reactor fuels, and non-destructive evaluation. After 40 years of almost exclusive use by the U.S. Navy, the U.S. Department of “I saw a lot of great technical Energy in 2007 had designated ATR and presentations,” Yang said. “It covered associated post-irradiation examination a whole spectrum of new, innovative facilities as a National Scientific User studies.” In 2009, Yang’s proposal Facility, allowing broader access to for post-irradiation examination of nuclear energy researchers. ceramics for stability in advanced fuel applications was one of four NSUF “It gave universities access to a lot of experiments to be selected. Other equipment and opened up partnership projects have included: opportunities,” said Allen, the first ATR NSUF director. As a member • characterization on Bor-60 neutron of Allen’s team, Yang oversaw the irradiated austenitic stainless steels assembly of capsules for irradiation in and cast stainless steel, ATR, labeling them and making sure • characterization of neutron they got to Idaho National Laboratory irradiated NF709 stainless steel safely and on time. using atom probe tomography, “He deserves a lot of credit for the • evaluation of ferrite decomposition work he did on the first experiment, in irradiated and aged duplex cast getting it done,” Allen said. stainless steels, As a graduate student, Yang had studied • low temperature Fe-ion irradiation metal matrix composite materials for of 15-15Ti steel in different thermo- car engines. His interest in nuclear mechanical states, and energy started after graduation. “If you • synergistic effects of thermal aging and look at the energy industry, nuclear is neutron irradiation in 304L welds.
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Yong Yang, INL Research Center 27 • Nuclear Science User Facilities •
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28 Transmission Electron Microscope, MaCS, CAES \ 2016 | ANNUAL REPORT
In 2016, Yang became chairman of The NSUF Users Organization is the NSUF Users Organization, which also teaming up with the American was set up in 2010 to provide a formal Nuclear Society, sponsoring and and clear channel for the exchange of presenting at its student conferences, information, advice, and best practices and encouraging current members to between investigators and NSUF help with recruiting through social “[The ATR National management. In this position, he has media applications such as Facebook turned his attention to what can be and LinkedIn. done to increase membership and Scientific User Facility] gave Allen said Yang is a great example of promote engagement. the type of professional the NSUF At the next Users Week in 2018, hopes to develop. “He’s a smart universities access to a lot Yang said he hopes to see the focus scientist, good at generating business, expanded beyond materials, capturing and a good mentor,” he said. of equipment and opened up a bigger audience. “I think this should The same year he became the NSUF be a central piece for nuclear R&D,” Users Organization chairman, Yang he said. partnership opportunities,” received his tenure and promotion Some objectives to bring this about to associate professor at University of include more scientific and technical Florida in 2016. In March 2017, the — Dr. Todd Allen, presentations to balance the educa- university’s training reactor received tion and training lectures, reaching its license renewal from the Nuclear the first ATR NSUF director out to the nuclear industry and Regulatory Commission, allowing the recruiting more of its leaders to training reactor to remain in operation speak. Live conferencing has also until March 2037. been suggested as a way to reach out For more information on the NSUF to partner facilities. Users Organization, please visit the NSUF website at https://nsuf.inl.gov.
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PROGRAM OVERVIEW
The NSUF: A Model for • Illinois Institute of Technology development activities based on Collaboration • Massachusetts Institute of Technology four main objectives that address The Nuclear Science User Facilities • North Carolina State University challenges to expanding the use of (NSUF) and its partner facilities nuclear power: • Oak Ridge National Laboratory represent a prototype laboratory that • Develop technologies and other utilizes a distributed partnership, with • Pacific Northwest National Laboratory solutions that can improve the reli- each facility bringing exceptional • Purdue University ability, sustain the safety, and extend capabilities to the relationship • University of California, Berkeley the life of current reactors. including reactors, beamlines, • University of Michigan • Develop improvements in the state-of-the-art instruments, hot cells, • University of Nevada – Las Vegas and equally important, expertise. affordability of new reactors to • University of Wisconsin These capabilities and people together enable nuclear energy to help meet create a nationwide infrastructure • Westinghouse Materials Center the administration’s energy security that allows the best ideas to be tested of Excellence. and climate change goals. • Develop sustainable nuclear fuel cycles. using the most advanced capabilities. This report contains details on new Through the NSUF, researchers capabilities brought into the NSUF in • Understand and minimize the risks of and their collaborators are building 2016, the evidence of the increasing nuclear proliferation and terrorism. on current knowledge to better research facilitated by the NSUF, and The NSUF research consortium understand the complex behavior of new tools and activities to propel addresses the first three of these materials and fuels in a nuclear reactor. nuclear research and development objectives. The NSUF does not conduct The NSUF’s partnership program in forward to meet energy reliability and classified work and all NSUF work is 2016 included eight universities, one security needs. Learn about the NSUF non-proprietary and intended for open research and education consortium, Nuclear Fuels and Materials Library literature publication, so applications three national laboratories, and and the Nuclear Energy Infrastructure to the NSUF research consortium one industry partner. The avenues Database, and how the robust NSUF have addressed only the first three of opened through these partnerships website continues to evolve to these objectives. Most of the research facilitate cooperative research across support new tools. Read about how contained in this report looks at either the country, matching people with the NSUF supports U.S. Department understanding the mechanisms of capabilities and students with mentors. of Energy (DOE) missions through radiation damage to materials and fuels The NSUF in 2016 included Idaho efforts like the 2016 NSUF Ion Beam or looks at materials and fuels for the National Laboratory (INL) and the Options Workshop, which led to a next generation of reactors. following institutions: prioritization of ion beam facilities according to their ability to support Take time to read through this report • Argonne National Laboratory U.S. Department of Energy Office of and familiarize yourself with the many • Center for Advanced Energy Nuclear Energy (DOE-NE) missions. opportunities and resources offered Studies (a research and education by the NSUF. For specific information consortium between Boise State NSUF Research Supports on DOE missions, go to http://www. University, INL, Idaho State DOE-NE Missions energy.gov/ne/mission. To learn University, University of Idaho, and As referenced in the 2010 DOE more about proposing a research University of Wyoming) Nuclear Energy Research and project, visit the NSUF website: Development Roadmap, DOE-NE http://nsuf.inl.gov. organizes its research and 30 2016 | ANNUAL REPORT
Analytical Chemistry Laboratory, CAES 31 Nuclear Science User Facilities
A TREMENDOUS SUCCESS CINR FOA
s stated in the Consolidated The initial offering in FY 2015 drew a Innovative Nuclear Research fair response with 31 pre-applications. A(CINR) Funding Oppor- Interest more than doubled in FY tunity Announcement (FOA), the 2016. After the dust settled from the U.S. Department of Energy Office of kick-off webinar and letter-of-intent Nuclear Energy (DOE-NE) conducts submittals, 67 pre-applications were crosscutting nuclear energy research submitted for the NSUF related work and development (R&D) and associ- scopes. About half of the pre- ated infrastructure support activities applications were invited to submit to develop innovative technologies full applications and, in the end, 12 that offer the promise of dramatically awards were made via the CINR FOA. improved performance for advanced The total access value of the NSUF reactors and fuel cycle concepts while awards was approximately $10 million also maximizing the impact of DOE and R&D funds associated with the Dan Ogden resources. DOE-NE funds research access totaled $4 million. activities through both competitive and Deputy Director The next CINR FOA cycle was initiated direct mechanisms, as required to best at the close of FY 2016 and the meet the Department’s needs. number of pre-applications more To support DOE-NE in maximizing than tripled, with 109 received. The its nuclear energy R&D portfolio, NSUF is hoping to increase our award the NSUF in fiscal year (FY) 2015 budget in FY 2017 – so stay tuned for transitioned from its historical call for the results! proposals to the CINR FOA. The CINR For information regarding the CINR FOA offers NSUF users a mechanism FOAs, please visit the NSUF website at to request R&D funding along with https://nsuf.inl.gov. NSUF access in a single proposal. The single proposal process eliminated user concerns regarding fragmented and leveraged proposals that many times resulted in partial awards, i.e., NSUF access without R&D funds – or worse, no awards.
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FY 2016 CINR Awards
Title PI Institution NSUF Utilization Effects of High Dose on Laser Welded, Janelle Purdue INL Materials and Fuels Complex Irradiated AISI 304SS Wharry University Westinghouse, CAES Microscopy and Characterization Suite Feasibility of Combined Ion-Neutron Zhijie Jiao University of ORNL Low Activation Materials Irradiation for Accessing High Dose Levels Michigan Development and Analysis Laboratory, Michigan Ion Beam Laboratory Fission Product Transport in TRISO Fuel Fei Gao University of Michigan Ion Beam Laboratory at the Michigan University of Michigan Irradiation Performance Testing of Jeffrey Colorado INL Advanced Test Reactor, INL Materials Specimens Produced by Commercially King School of Mines and Fuels Complex, CAES Microscopy Available Additive Manufacturing and Characterization Suite Techniques Radiation Enhanced Diffusion of Ag, Tyler Gerczak Oak Ridge Michigan Ion Beam Laboratory, ORNL Ag-Pd, Eu and Sr in Neutron Irradiated National High Flux Isotope Reactor PyC/SiC Diffusion Couples Laboratory Radial Heat Flux – Irradiation Synergism Yutai Oak Ridge ORNL High Flux Isotope Reactor, ORNL in SiC ATF Cladding Katoh National Low Activation Materials Development Laboratory and Analysis Laboratory Enhancing Irradiation Tolerance of Haiming Idaho State INL Advanced Test Reactor, INL Materials Steels via Nanostructuring by Innovative Wen University and Fuels Complex, CAES Microscopy Manufacturing Techniques and Characterization Suite Understand the phase transformation of Yong Yang University of Illinois Institute of Technology – MRCAT thermally aged and neutron irradiated Florida beamline at the Advanced Photon Source duplex stainless steels used in LWRs Irradiation Testing of LWR Additively Ronald Horn GE Hitachi INL Advanced Test Reactor, INL Materials Manufactured Materials Nuclear Energy and Fuels Complex, CAES Microscopy and Characterization Suite Effect of Gamma Irradiation on the Florence Vanderbilt ORNL Gamma Irradiation Facility Microstructure and Mechanical Properties Sanchez University of Nano-modified Concrete Correlative Atom Probe and Electron Phil Oak Ridge ORNL Low Activation Materials Microscopy Study of Radiation Induced Edmondson National Development and Analysis Laboratory Segregation at Low and High Angle Grain Laboratory Boundaries in Steels Role of minor alloying elements on long Julie Tucker Oregon State Wisconsin Tandem Accelerator Ion Beam range ordering in Ni-Cr alloys University
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RTE/BEAMLINE DEMAND INCREASES
RTE Overview beam [FIB], transmission electron The Nuclear Science User Facilities microscope [TEM], scanning electron (NSUF) Rapid Turnaround Experiment microscope [SEM], etc.), synchrotron (RTE) and Beamline awards provide an irradiation, ion beam irradiation, avenue to examine irradiation effects on or high performance computing. nuclear fuels and materials. Once started, Proposals are reviewed and awarded experiments typically are completed in three times per year. Proposals are two weeks or less. These awards allow reviewed, and scored for technical researchers to utilize an NSUF facility to merit, relevancy, feasibility, and then examine fuels or materials of interest for prioritized by total score. their research area. 2016 RTE Program Growth RTE proposals typically request post The NSUF RTE program has grown irradiation examination requiring significantly since its inception in use of instruments (focused ion 2010 and continued to grow in Jeff Benson Program Administrator 75
48 47 39
30 27 25 18 19 13 10 10 6 3 2010 2011 2012 2013 2014 2015 2016
RTE Proposals RTE Awards
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fiscal year (FY) 2016. The chart Summary illustrates the growth of the proposals In 2016, the NSUF has seen a and awards by year. significant increase in the number “Driving the increase in RTE/ of proposals and demand for access In FY 2016, the NSUF received 75 to partner facilities. As a result of the proposals from 24 different institu- Beamline Awards is strong demand – and with improved budgets tions. There were 28 more proposals – the NSUF RTE program has been received than from the prior year. successful in increasing the number of From the 75 proposals, the NSUF interest in the field of research awards for researchers (at no cost to selected 39 proposals for award to the researcher) to world-class capa- 18 different institutions. The number bilities to facilitate the advancement and the addition of a new of RTE awards in 2016 represents a of nuclear science and technology. 30 percent increase from 2015. Driving the increase in RTE/Beamline partner facility, the IVEM- The RTE program also saw significant Awards is strong interest in the field growth in the use of partner facilities. of research and the addition of a new The 2016 RTE awards requested access partner facility, the IVEM-Tandem Tandem Facility, in FY 2016.” to eight of the thirteen NSUF partner Facility, in FY 2016. facilities to perform experiments. The Please visit the NSUF website at https:// number of NSUF partners requested nsuf.inl.gov for up-to-date information for RTE awards in 2016 represents a on RTE and Beamline awards. 38 percent increase from 2015.
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Intermediate Voltage Electron Microscopy (IVEM)-Tandem Facility, Argonne National Laboratory (ANL) - Courtesy of ANL 36 2016 | ANNUAL REPORT
NEW NSUF PARTNER FACILITY IVEM-TANDEM
he Nuclear Science User beam, allowing in-situ irradiations Facilities (NSUF) welcomed during observation under controlled Tin fiscal year (FY) 2016 a new sample and diffracting conditions. partner facility, the Intermediate Capabilities include continuous Voltage Electron Microscopy (IVEM)- recording to provide real-time Tandem Facility at Argonne National observation of defect formation and Laboratory. The IVEM-Tandem Facility evolution during irradiation and well combines ion beam irradiation controlled experimental conditions capability with in-situ characterization (constant specimen orientation and using a transmission electron micro- area, specimen temperature, ion scope. A total dose of 100 dpa can be type, ion energy, dose rate, dose, and achieved in about a day. applied strain). A radiological facility, The IVEM is one of two similar the Irradiated Materials Laboratory facilities in the United States and (IML), located in the same building as is one of only five in the world. It the IVEM-Tandem, can receive, handle, has the unique ability to image the prepare, and store radioactive samples. changes in microstructure and defect For more information on the IVEM- formation during irradiation at high Tandem Facility, visit the NSUF website magnification. The IVEM interfaces at https://nsuf.inl.gov or the Argonne with an ion beamline incident from National Laboratory’s facility page at above at 30 degrees to the electron http://www.ne.anl.gov/ivem/.
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NUCLEAR FUELS and MATERIAL ONLINE LIBRARY
he Nuclear Science User Facili- back to ensure that information and ties (NSUF) Nuclear Fuels and materials are properly archived. The TMaterials Library went online in NSUF has prioritized: 2016 to establish another pathway for • documenting “tribal knowledge” research. The library is a collection of (long stored legacy material infor- specialized information, nuclear fuel mation, locations,pedigrees, etc.), and material specimens from past and ongoing irradiation test campaigns, • making materials inventories real-world components retrieved from accessible to researchers, and decommissioned power reactors, • including archived materials to and donations from other sources. It validate past and current analyses. includes irradiated and unirradiated The library has grown to approxi- samples in a wide range of material mately 6,000 specimens, up from types, from steel samples irradiated approximately 3,500 at its inception. Continued collaboration within the Kelly Cunningham in fast reactors to ceramic materials Nuclear Fuels and irradiated in the Advanced Test Reactor. nuclear community will expand the inventory by adding materials in line Materials Library Coordinator The Nuclear Fuels and Materials Library with DOE-NE’s current mission and is owned by the U.S. Department of future NE research needs. DOE-NE Energy’s Office of Nuclear Energy periodically issues Requests for Infor- (DOE-NE) and curated by the NSUF. mation to supplement the library’s Many of the samples are from previous offering by asking researchers to U.S. Department of Energy (DOE) provide information on: funded material and fuel development programs. Researchers can propose to • existing nuclear energy research analyze these samples in a post-irradi- materials and specimens that can, ation examination (PIE) only experi- potentially, be added to the Nuclear ment. Samples from the library may be Fuels and Materials Library, and used for proposals for open calls and • future needs for nuclear energy rapid turnaround experiments. related material to support ongoing As the NSUF program continues to nuclear energy challenges as well grow, so will easily accessible NSUF as future research advancements in research tools like the Nuclear Fuels nuclear energy. and Materials Library. Expanding the The library can be accessed via the Library’s inventory means reaching NSUF’s website at https://nsuf.inl. gov or directly via the Nuclear Energy Infrastructure Database at https://nsuf- infrastructure.inl.gov/browse/materials.
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Series of sample holders in a Containment Box, Hot Fuels Examination Facility (HFEF), MFC, INL 39 Nuclear Science User Facilities
ION BEAM CAPABILITIES NSUF AT WORK
hen U.S. Department of Thirty-three members of the ion Energy Office of Nuclear beam community attended the WEnergy (DOE-NE) leaders invitation-only workshop. Attendees needed expert input on how to represented 15 operating and prioritize the importance of domestic proposed ion beam facilities, six ion beam irradiation capabilities, they DOE-NE research and development called the NSUF – and NSUF ion beam (R&D) programs, the Electric Power research capabilities experts answered Research Institute, and the chairs of the call. the NSUF Users Organization and the NSUF Science Review Board. The NSUF, at the request of DOE-NE, Three members of the sponsoring held an Ion Beam Workshop in agency, the Office of Science and March 2016 in Idaho Falls, Idaho. Technology Innovation (DOE-NE-4), The workshop was organized at the also attended the workshop. direction of DOE-NE to develop a set Brenden Heidrich of recommendations for prioritizing Consensus Criteria Capabilities Scientist domestic ion beam irradiation The workshop participants developed capabilities available to researchers. by consensus a list of ten criteria Domestic ion beam capabilities are against which to compare the various focused on the support of nuclear ion beam facilities. The criteria are energy research and development, both tied directly to ion beam capabilities of which are key to DOE-NE’s missions. that support DOE-NE’s mission and thus will help DOE-NE understand the DOE-NE intends to use the input priorities for future federal decisions. provided by the workshop when deciding how to best use NSUF ion beam capabilities, instruments, and facilities. A cross section of the ion beam community participated in the workshop.
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Triple Beam Target Chamber, Michigan Ion Beam Laboratory, University of Michigan 41 Nuclear Science User Facilities
Michigan Ion Beam Laboratory, University of Michigan
COMBINED CRITERIA
C1 Viability for the capability to extend our understanding toward accurately simulating nuclear irradiation conditions (neutrons or fission fragments)
C2 Ability of the facility to provide a variety of ion irradiations (ion types, energies, multiple beams, etc.)
C3 Ability of the facility to provide a variety of well-controlled target environments and conditions
C4 Ability of the facility to collect and analyze properties of materials and/or perform microstructural characterization data on-site
C5 Ability of the facility to collect and analyze properties of materials and/or perform microstructural characterization data in-situ
C6 Current or potential productivity of the facility (e.g., fewer experiments but high-impact experiments or high volume sample throughput)
C7 Unique capabilities of the facility, including any new technology that the capability has to close technological gaps
C8 Ability of the facility to handle radioactive materials (structural materials and/or fuels) in the beams and elsewhere on-site
C9 Ability of the facility to produce quality-level data that can support licensing as well as verification and validation of modeling and simulation
C10 Ability of the facility to produce results that meet the needs of the DOE-Office of Nuclear Energy (including cross-cutting programs) and the nuclear energy industry
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Participants from ion beam users • The Center for Materials under • Texas A&M University – and DOE-NE R&D programs first Extreme Environment Facility Ion Beam Laboratory presented information on capabilities at Purdue University focuses on • University of Michigan – Michigan and needs to begin the consensus surface science of materials and Ion Beam Laboratory (MIBL) building process. The ion beam facility utilizes much lower energy ions • University of Tennessee – representatives then shared their than the others. Ion Beam Materials Laboratory respective presentations. Following • The Edwards Accelerator • University of Wisconsin – this informative discussion, workshop Laboratory at The Ohio University Ion Beam Laboratory. participants buckled down and is primarily engaged in nuclear The NSUF will proceed in facilitating assessed each ion beam facility against data measurement and not in the DOE-NE’s effective use of ion beam the 10 criteria. irradiation effects on materials. capabilities by 1) producing an Workshop participants recognized • The Idaho Accelerator Laboratory Ion Beam Utilization Roadmap and early on that ion beam facilities have at Idaho State University is a 2) evaluating additional ion beam individual focus areas and objectives multipurpose facility that supports a capabilities through the NSUF and thus may have significantly wide variety of research endeavors. Partner Facility application process different designs. Since form follows These three facilities should not from institutions interested in joining function, the differing objectives were be judged in the same manner as the consortium. delineated by participants. the others. For the former, the NSUF will Ion Beam Facility Categories DOE-NE R&D Ion Beam Capabilities assemble a voluntary team of ion Workshop participants reviewed and Beyond this, the remaining eight beam experts whose mandate will be categorized 15 ion beam facilities. currently operating facilities all to prepare a report describing current Proposed Ion Beam Capabilities provide vital support to nuclear and potential future contributions of Four facilities were proposed to materials researchers. The individual ion beam technologies to address the be built in the future to provide capabilities of these eight facilities technical and regulatory challenges expanded ion beam capabilities, differ based on their particular of the nuclear energy community for including combining ion beam missions. Three facilities have the advancement and implementation irradiation capability with in-situ – or will have soon – in-situ of nuclear energy technologies characterization with an X-ray source: characterization capabilities that that are part of the mission of combine ion irradiation with a DOE-NE. The report should establish • Argonne National Laboratory (ANL) transmission electron microscope recommendations and their impacts – Extreme Materials Beam Line (IVEM, I3TEM, and MIBL (pending)). for DOE-NE and its programs to use at (XMAT) Eight currently operating ion beam their discretion in establishing future • Brookhaven National Laboratory facilities that either already support directives and priorities. (BNL) – Ion X-Ray Beam (IXB) DOE-NE R&D needs through the For the latter, the NSUF will review • BNL – Ion Irradiation Facilities and NSUF or could eventually support applications under the criteria of Capabilities at the BNL Accelerator needs through the NSUF: whether the capability is unique with Complex – BLIP BLAIRR • ANL – Intermediate Voltage Electron respect to what is already part of the • Massachusetts Institute of Microscope (IVEM) NSUF or if the capability is in such Technology (MIT) – MIT Nuclear high demand that additional capability • Los Alamos National Laboratory – Materials Laboratory is needed in the NSUF in fulfilling the Ion Beam Materials Laboratory Multipurpose Ion Beam Capabilities mission of DOE-NE. Site visits and Workshop participants recognized • Lawrence Livermore National capability inspections will be part of that three facilities had primary Laboratory – Center for Accelerator these evaluations. focuses outside of materials Mass Spectrometry irradiations supporting DOE-NE’s key • Sandia National Laboratories – mission areas: In-Situ Ion Irradiation Transmission Electron Microscope (I3TEM)
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DISTRIBUTED PARTNERSHIPS
Pacific Northwest National Laboratory
Center for Advanced Energy Studies Massachusetts Institute University of of Technology INL Wisconsin, Madison University of Michigan
Illinois Institute University of of Technology Westinghouse California, Berkeley Purdue University Argonne National Laboratory University of Nevada, Las Vegas
North Carolina Oak Ridge National State University Laboratory
PIs/User Institutions Partners (As of 2017)
Partner Facilities
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HFEF, MFC, INL
User Institutions
Arizona Michigan Texas Arizona State University Michigan State University Texas A&M University University of Michigan California Utah University of California, Berkeley Missouri Utah State University University of California, University of Missouri Virginia Santa Barbara Nevada Virginia Commonwealth University Colorado University of Nevada – Las Vegas Washington Colorado School of Mines New Mexico Pacific Northwest Florida Los Alamos National Laboratory National Laboratory Florida State University North Carolina Wisconsin University of Central Florida GE Hitachi Nuclear Energy University of Wisconsin University of Florida North Carolina State University Australia Idaho Ohio Australian Nuclear Science and Boise State University The Ohio State University Technology Organization Idaho National Laboratory Idaho State University Oregon United Kingdom University of Idaho Oregon State University Oxford University University of Liverpool Pennsylvania Illinois University of Manchester Argonne National Laboratory Drexel University Illinois Institute of Technology Tennessee University of Illinois Oak Ridge National Laboratory Massachusetts University of Tennessee Massachusetts Institute of Technology Vanderbilt University
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46 NRAD Reactor Pool, MFC, INL 2016 | ANNUAL REPORT
NSUF AWARDED PROJECTS
This section contains reports on projects awarded through the NSUF and completed in FY 2016.
Flashback: NSUF History
n Advanced Test Reactor and would expand the scientific National Scientific User Facility foundation for fuels and materials to AProgram could serve a key role improve nuclear energy systems. It in reestablishing the U.S. scientific would also align with the President’s and nuclear industrial base that is American Competitive Initiative needed for building a new generation and strengthen nuclear engineering of nuclear power plants in the United education in the United States. States and in ensuring the safety of – U.S. Department of Energy Memo: the existing nuclear power plants. Designation of INL ATR as a National Establishing the Advanced Test Reactor Scientific User Facility as a National Scientific User Facility will help reassert U.S. leadership April 13, 2007 in nuclear science and technology
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Characterization of CANDU Core Internals via Small Scale Mechanical Testing Peter Hosemann – University of California, Berkeley – [email protected]
The application of the Focused Ion Beam (FIB) to extract micro-scale samples of in-service components with pre-selected microstructures (i.e., individual grain boundaries) is a powerful technique that allows for insight into real-time mechanical testing observation of failure mechanisms, and the FIB research conducted at the MFC and the University of California, Berkeley moves this method to the forefront of the nuclear scientific community.
ANada Deuterium Uranium degradation rates are essential for long (CANDU) Inconel X-750 term prediction of mechanical failure Cspacers incur higher doses through appropriate models. Micro- and He/dpa ratios than light water scale testing will provide insight reactor (LWR) materials. They into the temperature dependence separate hot pressure tubes from of embrittlement at operating cold calandria tubes, preventing temperatures that can then be low-pressure moderator from applied to components subject to He contacting hot pressure tubes. embrittlement in all reactors. Segments at 330°C exhibit lower Project Description strength and ductility than 200°C The objective of this research was segments. Lower temperature parts to obtain quantitative mechanical support fuel channels, preventing properties of Inconel X-750 CANDU contact between hot and cold tubes. core components at two different Weakening and embrittlement occur irradiation temperatures and doses. after 2/3 of the tubes’ expected A new in-situ scanning electron lifetime. Inspected springs exhibited microscope (SEM) small-scale intergranular failure upon handling. mechanical test, namely lift-out Quantification of changes in failure three-point bending, was developed stresses as compared to virgin and executed on active CANDU core materials is needed. Embrittlement components. Given the difficulties in occurs in Ni alloys with irradiation manufacturing and testing multiple temperatures > 500°C, but there are specimens to obtain good statistics few instances of low temperature from active bulk spring coils, the effects. Failure mechanisms and
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Figure 1. Electron Backscatter Diffraction (EBSD) scans of 250 μm x 250 μm squares of the inner edge, center, and outer edge regions of an Inconel X-750 flat spring. EBSD orientation map grain analysis produces an average overall grain size of 8.5 ± 2.9 μm and indicates grain elongation in the tangential direction.
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Figure 2. (a) cross-section of an reproduceability of testing that (increased displacement damage and Inconel X-750 spring showing provides quantitative yield-strength helium and hydrogen content) and focused ion beam (FIB) milled foils of material taken from both edge values and a real-time look at can be used as a predictive model for and center regions (b) resulting deformation processes makes this future effects that will occur in LWR bending beam structures cut an exciting technique. This specific structural materials. into the large lift-out foil which project was to conduct micro-scale has already been removed from Accomplishments mechanical testing on annulus the bulk spring (c) side view of a Large foils of active Inconel X-750 spacers irradiated at 180 and 300°C finished three-point bend specimen spacers were fabricated on the focused (d) top view of a completed three- in service for approximately 14 and ion beam at the Materials Fuels point bend specimen. 19 equivalent full-power years to Complex (MFC) in Idaho under the quantify differences in mechanical direction of Colin Judge and Cameron properties. This research supports Howard, and shipped to the University efforts to make the micro-scale of California Berkeley nuclear materials investigation and testing of nuclear laboratory. This research was conducted core structural components more primarily by Cameron Howard and reproduceable, quantitative, and facilitated in large part by staff at cost-effective by minimizing the MFC, including microscopist James use of hot cells and developing W. Madden, staff scientist Brandon D. new in-situ small-scale mechanical Miller, and project director Collin J. testing techniques. Because these Knight. These foils were subsequently CANDU core components are sectioned into individual specimens nickel superalloys, they incur more and an in-situ lift-out three-point pronounced radiation damage effects bending test technique was developed
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Figure 3. Pre-test Electron Backscattered Diffraction (EBSD) on the top surface of a representative three-point bend specimen including an Inverse Pole Figure (IPF) grain orientation map in the tensile stress direction on the outer fiber of the specimen, hkl orientation of individual grains, misorientation angles between two grains, grain rotation within each grain, and Schmid factor map indicating the likelihood of deformation slip along the most preferred slip system within each grain.
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Figure 4. Representative flexural stress-strain curves calculated for the midpoint at the outer fiber of the (a) center and (b) edge specimens according to three-point bend theory for each irradiation condition. Loading curves plotted in terms of critical resolved shear stress (CRSS) can be seen for the center specimens in (c) and edge specimens in (d).
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and applied by Cameron Howard and Future Activities Steven Scott Parker to components A manuscript for the Journal of irradiated at 180 and 300°C in Nuclear Materials has been drafted service for approximately 14 and 19 with the intention of submission and equivalent-full-power years as well as publication in the near future on the Access to the MFC facility to non-irradiated control specimens. novel in-situ three-point bending technique and the results found This work was performed in the FEI for these core components. Newly Quanta Dual Beam SEM/FIB in the has provided unprecedented developed push-to-pull tensile testing University of California, Berkeley to assess the grain boundary strengths nuclear materials laboratory. In addi- of these components remains ongoing capabilities for large-scale tion, investigations of pre-existing and will serve as the remainder of the cold-work effects created during Ph. D. thesis for Cameron Howard. spring coil production and how work on in-service nuclear these may change over the course Publications of in-service time and irradiation [1.] C. Howard, et al., “Mechanical structural materials temperature, as suggested by Malcolm Characterization of In Service Griffiths and Steven Xu, were Inconel X-750 Annulus Spacers,” performed for samples of all irra- 146th Annual Meeting of the — Cameron Howard, diation conditions by extracting and Minerals, Metals, and Materials Ph.D. Researcher, Department testing material from both the edge Society, February 2017. of Nuclear Engineering, Nuclear and center regions of the spacers. *See additional publications from other years in the Media Library on the Materials Group, University of NSUF website. California, Berkeley Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Idaho National Laboratory Electron Microscopy Laboratory University of California, Nuclear Materials Laboratory Berkeley Collaborators Canadian Nuclear Colin Judge (Collaborator) Laboratories Kinectrics Inc. Steven Xu (Collaborator) Queen’s University Malcolm Griffiths (Collaborator) University of California, Peter Hosemann (principal investigator), Berkeley Cameron Howard (Co-Principal Investigator), Steven Scott Parker (Collaborator)
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Atom Probe Characterization of Phase Separation During Age Hardening of a U-6wt.%Nb Alloy Clarissa Yablinsky – Los Alamos National Laboratory – [email protected]
Figure 1. Tip reconstructions for aging times of 10 minutes at 500°C, 100 minutes and 500°C, and 10000 minutes at 500°C. The non-lamellar precipitate structures all contain interconnected alpha-U precipitates, which coarsen with age, of varying widths and orientations.
Project Description Accomplishments Understanding The technical objective of this study Clarissa Yablinsky was able to decomposition was to probe an aged material accomplish the microscopy and atom mechanisms in using an instrument capable of probe for one of the four samples metallic fuel will help giving information on structure proposed, rounding out a set of 3 with performance and chemistry. The two-phase aging conditions: 10 min at 500°C prediction over the microstructure of the U-6Nb alloy (completed this fiscal year [FY]), 100 lifetime of a reactor. undergoes aging decomposition min at 500°C, and 10000 minutes during heat treatments at temperatures at 500°C (completed in previous used in reactors and is a simple alloy year outside of Nuclear Science User to probe phase transformations, Facilities [NSUF]). General trends kinetics, and age-hardening were observed with aging: the Nb mechanisms. Metallic uranium segregation to the matrix was greater fuel will be necessary in advanced with increased aging and the U reactors to meet the fissile-atom precipitate increased in concentration density requirements of reactors as the Nb segregated. This increase while maintaining low enrichment in partitioning relates to the energy that policy demands. Understanding released during the decomposition; decomposition mechanisms and thus, the same trend is seen for the underlying kinetics within the extent of partitioning, delta C, where operating temperature regime is delta C increases with aging time. The necessary for performance prediction Center for Advanced Energy Studies for reliability, safety, and life extension (CAES) staff was instrumental in for new reactors.
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Figure 2. The data added at 500°C in the NL3 regime is presented with orange squares. The evolution in Nb partitioning throughtout the aging, moving from an NL3 decomposition mechanism, to the DP, and finally to DC, shows the chemical evolution of the metallic fuel with time.
The CAES MaCS facility is well run and was an excellent performing the microscopy due to complete set is finished, we will their radiological training and careful do further analysis of the kinetics place to do microscopy and atom approach to sample handling. and structure and begin writing a paper that incorporates the results Future Activities with previous hardening and probe for my uranium project. Because of shipping issues, we decomposition mechanism data. were unable to finish the other three samples in FY 2015. After the — Clarissa Yablinsky, Scientist
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Los Alamos Clarissa Yablinsky (principal investigator), National Laboratory Robert Hackenberg (collaborator), Amy Clarke (collaborator)
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Si-Ni-Mn Clustering in Irradiated Fe-9Cr Oxide Dispersion Strengthend Alloy Janelle P. Wharry – Purdue University – [email protected]
Figure 1. Atom probe tomography xide dispersion strengthened steels are based upon the b.c.c. Fe-Cr (APT) reconstructed tips showing (ODS) alloys are nanofea- alloy system, it is unsurprising that Si-Ni-Mn clustering on oxide tured materials, having grains Si, Ni, and Mn would also cluster in nanoparticles in model Fe-9Cr O irradiated with (a) 5 MeV Fe++, of diameter ~250 nm and containing ODS alloys. 100 dpa, 400°C, (b) 2 MeV a dispersion of oxide nanoparticles. Project Description protons, 3 dpa, 500°C, and (c) The fine grains and oxide nanopar- neutrons in ATR, 3 dpa, 500°C. The objective of this project is to ticles provide the alloy with high understand the role of Si, Ni, and Mn strength at elevated temperatures and clustering in irradiated ODS alloys. dimensional stability under irra- Specifically, we test the hypothesis that diation, making ODS alloys leading there is a co-evolution of Si-Ni-Mn candidates for structural components rich clusters (which nucleate under in fusion and advanced fission reac- irradiation) and pre-exisitng oxide tors. Most post-irradiation evaluation nanoclusters under irradiation. In this (PIE) experiments of ODS alloys have project, we first conducted proton focused on evaluating the stability of and Fe2+ self-ion irradiations to the oxide nanoparticles and several several doses between 1 and 100 researchers have observed instability displacements per atom (dpa) at of these nanoparticles under irra- 500°C on a model Fe-9Cr ODS alloy. diation at moderate temperatures. We also access a 3 dpa, 500°C neutron However, there have been no specific irradiated specimen of the same alloy investigations into the clustering of heat through the NSUF Nuclear Fuels Si, Ni, and Mn in ODS alloys. These and Materials Library. We carried out minor elements have been found to microstructure characterization by cluster readily in other b.c.c. Fe-Cr atom probe tomography (APT) for the alloys, including commercial ferritic/ nanoscale cluster analysis, along with martensitic (F/M) steels. Since ODS complementary transmission electron microscopy (TEM) to characterize dislocations, loops, carbide
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precipitates, and voids. All of these Accomplishments experiments were conducted at the The atomic level resolution of Microscopy and Characterization Suite APT with Interactive Analysis and (MaCS) at the Center for Advanced Visualization Software (IVAS) Energy Studies (CAES). cluster analysis enabled both the characterization of the irradiation This project will contribute to the induced dissolution of oxide scientific community in numerous nanoclusters and the irradiation ways. First, this project will help us induced formation of Si-, Ni-, Oxide gain a deeper understanding of the and Mn-rich clusters. The three- nanoparticles mechanisms of Si-Ni-Mn clustering dimensional reconstructions of the co-evolve with in b.c.c. Fe-Cr alloys. More specifically, neutron-, proton-, and self-ion- Si, Mn, and Ni this project will help us understand irradiated specimens all exhibit radiation induced the role of Si-Ni-Mn clustering in clustering of Ti, O, and Y atoms segregation in the irradiation stability of oxide along with TiO, YO, FeO, and CrO ODS alloys. nanoparticles in ODS steels. Stability compounds at coincident locations of these oxide nanoparticles is critical in the matrix. There is also visual to the long-term material integrity of evidence of clustering among the ODS alloys in cladding and structural Si, Mn, and Ni atoms at the same components in fission and fusion locations. Multiple localized electron reactors. Second, this project presents atom probe (LEAP) tips were analyzed a rare and unique opportunity to from each of the as-received and compare neutron, proton, and self-ion irradiated specimens. Representative irradiation effects in identical heats of atom distribution maps, as created by a model Fe-9Cr ODS alloy at identical APT analysis and 3D reconstruction, irradiation temperatures and doses. This are shown in the attached figures. comparison offers great opportunity Quantitative chemical analysis, to help us understand fundamental enabled by the APT IVAS software, differences in the creation of confirms the visual evidence of Si, irradiation damage between neutrons, Mn, and Ni clustering. For example, protons, and self-ions. Third, results of the fraction of all detected Si, Mn, and this project will be relevant to all ODS Ni atoms that are found in clusters and other nanostructured alloys based (i.e. percent clustered) increases with on the b.c.c Fe-Cr matrix, which are of irradiation. In addition, the in-cluster growing interest to the U.S. Department composition of Si, Mn, and Ni of Energy Office of Nuclear Energy due increase with all types of irradiation, to their enhanced radiation resistance. while the matrix composition of Si Last, this project will enable a graduate decreases, further affirming that these student to utilize state-of-the-art ion species cluster during irradiation. beam irradiation techniques toward developing his thesis.
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The clustering of Si, Mn, and Ni is a The second possibility considered notable irradiation induced chemistry is that the Mn and Ni form silicide change. The formation of similar compounds and precipitate out of clusters containing Si, Mn, and Ni solution. Although all of these silicides is often reported in F/M steels such have a negative enthalpy of formation, as T91, HCM12, and HT9 and in these enthalpies are less favorable than austenitic stainless steels, but rarely in those of the oxides considered in the ODS steels. Several cluster formation first possible mechanism. Further- mechanisms have been proposed: more, if silicide formation were the primary mechanism for Si, Mn, and • Si, Mn, and Ni form oxide phases Ni clustering in ODS and F/M steels, such as SiO , Mn O , or NiO and 2 3 4 it would be expected that Mo would nucleate in conjunction with the also cluster in other F/M steels due existing oxide phases. to the negative Mo-silicide forma- • Si, Mn, and Ni form silicides such as tion enthalpy, yet this has not been Mn Si or Ni Si and nucleate as their 4 7 3 2 observed in irradiated F/M alloys. own precipitates, independent of the Thus, silicide formation is not likely existing oxides. the primary mechanism of Si, Mn, and • Si, Mn, and Ni diffuse towards sinks Ni clustering in ODS and F/M steels (such as oxides) due to radiation induced segregation (RIS). Finally, the possibility of RIS is consid- ered as the driving mechanism for Si, The first possible mechanism must Mn, and Ni clustering. Si, Mn, and Ni consider the enthalpy of formation are found in higher concentrations of the Fe, Cr, Y, Ti, Si, Mn, and Ni within the oxides following irradia- oxides relevant for 9-Cr ODS. All of tion. These same species are known these elements have a high affinity for to segregate toward grain boundaries oxygen, with the Si and Mn having in commercial F/M and austenitic enthalpy of oxide formation on the stainless steels. Thus, the RIS mecha- same order as that of Fe, Cr, and Ti. nisms reported in literature appear to Yet because Si, Mn, and Ni oxides be consistent with the solute enrich- or clusters are not present in the ments at oxides observed in this study, as-received condition, their clustering suggesting that the clustering of Si, Mn, is irradiation induced. In addition, and Ni is the likely result of RIS toward the oxide formation mechanism does existing point-defect sinks within the not explain why Si, Mn, and Ni also matrix, such as oxide nanoclusters. cluster upon irradiation in other F/M and austenitic stainless steels that This work was performed primarily by do not contain pre-existing oxide Matthew Swenson and Corey Dolph, compounds. Therefore, this is not under the research advisorship of likely to be the primary mechanism of Janelle Wharry. At CAES, the students Si, Mn, and Ni clustering. were assisted by Yaqiao Wu, Joanna Taylor, Alyssa Bateman, and Jatuporn
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Burns. At the Michigan Ion Beam nanoparticles in b.c.c. Fe-Cr alloys: Laboratory at the University of current understanding and future Michigan, the students were assisted by directions.” Submitted manuscript. Ovidiu Toader , Fabian Naab, and the [3.] M. J. Swenson and J. P. Wharry. graduate students employed there. “Collected data set size consid- Future Activities erations for atom probe cluster Our future work involves developing analysis.” Microscopy & Microanalysis a rate theory model to predict the 22.S3 (2016) 690. irradiation evolution of oxide and [4.] C. K. Dolph, D. J. DaSilva*, M. J. Si-Mn-Ni nanoclusters. This model Swenson, and J. P. Wharry. “Plastic will consider the RIS mechanism as zone size for nanoindentation of the driver of Si, Mn, and Ni clustering irradiated Fe-9wt% Cr ODS al- on existing oxides, and will predict loy.” Journal of Nuclear Materials 481 the long-term co-evolution of the (2016) 33. *undergraduate Si-Mn-Ni-enriched oxide clusters. [5.] M. J. Swenson, C. K. Dolph, and Publications J. P. Wharry. “The effects of oxide [1.] M. J. Swenson and J. P. Wharry. evolution on mechanical proper- “Standardizing atom probe cluster ties in irradiated 9wt% Cr ODS analysis methods: voltage and alloy.” Journal of Nuclear Materials 479 reconstruction considerations.” (2016) 426. Submitted manuscript. *See additional publications from other [2.] J. P. Wharry, M. J. Swenson, and years in the Media Library on the K. H. Yano. “A review of the irradi- NSUF website. ation evolution of dispersed oxide
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 Facility University of Michigan Michigan Ion Beam Laboratory Collaborators Boise State University Janelle Wharry (principal investigator), Matthew Swenson (collaborator), Corey Dolph (collaborator)
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Microstructural and Nanomechanical Characterization of a Lanthana-Bearing Nanostructured Ferritic Steel Irradiated with High Dose Iron Ions Indrajit Charit – University of Idaho – [email protected]
dvanced reactors need high Project Description performance materials to serve The project was geared toward Aunder harsh service conditions investigating 14LMT samples exposed such as higher temperature, higher to higher self-ion irradiation doses radiation doses, and extremely corro- (up to 400 dpa) and understanding sive environment. Nanostructured the effects of radiation damage doses. ferritic steels (NFS) are such a class of No irradiation task was included in Development of the materials, produced via mechanical the scope of this Rapid Turnaround new 14LMT alloy with alloying (MA) of the elemental (or Experiment (RTE) project because excellent radiation pre-alloyed) metallic powder, typi- the ion irradiation work has already resistant property may cally incorporating nanosized yttria been performed at the Texas A&M Ion pave the way for using powder, followed by a traditional Beam Laboratory led by Professor Lin high performance fuel consolidation process such as hot Shao. The ion irradiation parameters cladding and structural extrusion or hot isostatic pressing used are summarized as follows. materials for advanced (HIP). They are potential materials for Ion type: Fe2+ ion; ion energy: 4 nuclear reactors. advanced fuel cladding and structural MeV; irradiation mode: defocused; materials applications. The perfor- dose: 100, 200, 300, and 400 mance of NFS is largely determined dpa; dose rate: around 10−4 dpa/ by ultra-high-number density of second; irradiation temperatures: nano-sized oxide particles, which are 748 K. Furthermore, the initial dispersed throughout the microstruc- microstructure of the 14LMT alloy ture and stable at high temperatures. A has been thoroughly characterized new NFS, known as 14LMT (Fe-14Cr- by transmission electron microscopy 1Ti-0.3Mo-0.5La2O3, wt.%), was (TEM) and atom probe tomography recently developed by the principal (APT) in CAES MaCS. investigator’s group and his project For the post-irradiation examination collaborators. The 14LMT alloy uses portion of the project, four samples, lanthana in place of traditionally used each irradiated at 748 K, were exam- Y O . Spark plasma sintering (SPS) 2 3 ined. The irradiated specimens are was used to consolidate the mechani- studied for microstructural characteris- cally alloyed powder. tics and mechanical properties. Task 1. Preparation of APT and TEM specimens by focused ion beam (FIB) at MaCS.
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Figure 1. Transmission electron microscopy images of 14LMT alloy irradiated by ferrous ions to different ion-irradiation doses at 748 K.
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Figure 2. Three-dimensional reconstructed atom probe tomography maps of 14LMT alloy specimen irradiated by ferrous ions to 300 dpa at 748 K.
Task 2. Microstructural characterization Accomplishments of the prepared specimens. TEM studies The goal of the project was to were carried out on the prepared TEM examine the microstructure and specimens using the Tecnai TF30-FEG mechanical properties of the 14LMT S-Twin STEM to study the ion irradi- alloy irradiated with different ated microstructure with particular radiation damage doses (100–400 attention to both the irradiation dpa). Ion irradiation experiments on induced damage formation and the the 14LMT specimens were carried morphology and chemical analysis out by Dr. Lin Shao and his graduate of the nanometric particles. The APT student, Lloyd M. Price, at the Texas studies, conducted using the Cameca A&M University. Jatuporn Burns LEAP 4000X HR, provided information helped with the preparation of TEM on any change in their size, number and APT specimens using the FIB density, and composition as a function available at CAES-MaCS. Dr. Yaqiao Wu of dpa and irradiation temperature. helped the graduate students (Somayeh Pasebani and Ankan Guria) Task 3. Nano-indentation testing. perform the TEM experiments and APT Heavy ion irradiation led to only about analyses of the irradiated specimens a micron thick surface damage layer. of 14MLT. This research was primarily Hence, the nano-indentation tech- conducted by graduate students nique served as an effective method to Somayeh Pasebani and Ankan Guria. characterize mechanical property, such Joanna Taylor was instrumental in as elastic modulus and hardness of the facilitating our access to MaCS. ion irradiated damage layer. A Hysitron TI-950 Tribo-indenter available in MaCS was used for these experiments.
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Future Activities [3.] S. Pasebani*, A. Guria*, J. Burns, All the experimental activities have Y. Wu, I. Charit, D. P. Butt, It was a wonderful been completed. Some data analyses J. L. Cole, L. Shao and L. Price, are still in progress. “Microstructural and Nanome- chanical Characteristics of an opportunity for us to use the Publications Ion-Irradiated Lanthana-Bearing [1.] S. Pasebani, I. Charit, Y. Wu, Nanostructured Ferritic Steel,” J. Burns, K. N. Allahar, D. P. Butt, advanced tools/techniques Accelerated Materials Evaluation J. I. Cole, and S. F. Alsagabi, “Lan- for Nuclear Application Utilizing thana-Bearing Nanostructured Test Reactors, Ion Beam Facilities Ferritic Steels via Spark Plasma available at MaCS to achieve and Integrated Modeling, TMS Sintering,” Journal of Nuclear Materials Annual Meeting, held Feb. 14–18, 2016 470 (2016), pp. 297–306. at Nashville, TN. our project objectives. [2.] S. Pasebani, I. Charit, D. P. Butt, *See additional publications from other J. I. Cole, Y. Q. Wu, J. Burns, “Sinter- years in the Media Library on the — Indrajit Charit, ing Behavior of Lanthana-Bearing NSUF website. Nanostructured Ferritic Steel Con- Associate Professor, Department solidated via Spark Plasma Sinter- of Chemical and Materials ing,” Advanced Engineering Materials Engineering, University of Idaho 18.2 (2016), pp. 324–332.
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Boise State University Jatuporn Burns (co-principal investigator), Yaqiao Wu (collaborator) Texas A&M University Lin Shao (co-principal investigator) University of Idaho Indrajit Charit (principal investigator), Ankan Guria (team member - student), Somayeh Pasebani (team member - student)
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Irradiation Effects on Structure and Properties of LWR Concrete Chris Wetteland – University of Tennessee – [email protected]
Figure 1. Optical microscope image at 50, 100, and 150× magnification shows Accelerated aging experiments in concrete may offer insight discoloration and cracking in into the longevity of this crucial reactor building material. the nanoconcrete surface. This flux used in this irradiation was 5 × 1013 protons/cm2 and resulted in significant volatilization from the surface. he long-term stability and concrete recipes for future plants and performance of Portland cement storage containers. The experiments Tconcrete in nuclear power further establish considerations for plants is of concern as little opera- accelerated irradiation studies of tional or experimental data exist to concrete, which may be required due aid regulators in extending operating to the hydrous nature of the material. licenses. More complete knowledge Project Description of performance in radiation environ- The technical objectives of the research ments will determine concrete’s role are to understand the radiation in setting the upper limits for lifetime tolerance of concrete and how to extensions. In the awarded project, perform more-detailed accelerated- concrete, aggregate, and paste samples irradiation experiments in the future. were irradiated with energetic protons Most accelerated-aging experiments to simulate radiation damage. Volatile using accelerators require the target loss during irradiation was monitored materials to be stable in a vacuum with a mass spectrometer to determine environment; this is true for nearly all the ideal conditions to irradiate the metal and ceramic materials. However, concrete and concrete components. due to the hydrous nature of concrete, Samples were examined with optical it requires extensive pump-down times and electron microsope post irradia- prior to performing any irradiations. tion to determine the degree of surface The hydrous nature further complicates damage. Collected results were used to experiments because using the most determine possible radiation induced modest of beam fluxes can result in degradation in the current fleet, as well vacuum pressure changes two orders as aid in developing radiation tolerant of magnitude and greater. Changes
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Figure 2. Irradiation of a limestone disk using 2 MeV protons. Limestone (calcite) exhibits a strong luminescence in the visible spectrum during proton irradiation.
The series of irradiation experiments we performed on concrete and its aggregates are some of the first of their on this magnitude can cause damage future researchers examine radiation to internal accelerator and vacuum effects in concrete and its individual kind. This is the first step components and trigger safety valves components (aggregate and cement), during an experiment. Because of these these preliminary experiments will be restraints, experiments were conducted vital in designing accelerated aging in performing accelerated to determine the optimal experimental studies. Furthermore, these types conditions, including sample of studies will aid in the materials aging studies in this complex mounting, vacuum requirements, and selection for future reactors. This is beam currents, to perform accelerated particularly true in the selection of aging experiments. aggregate products in order to limit materials system. potential radiation accelerated alkali– As the U.S. reactor fleet ages and silica reaction (ASR). receives extensions for operating — Chris Wetteland, outside the intended lifespan, it is Accomplishments critical to understand how the Concrete irradiations are extremely Lecturer, University of Tennessee concrete structural components difficult. The difficulties arise in respond to long-term radiation limiting damage to the concrete exposure. The research in this arising from conditions that are Nuclear Science User Facilities (NSUF) outside the normal equilibrium sponsored study is the first step conditions in which the structure in qualifying concrete to perform resides, e.g., atmospheric pressure. beyond its intended lifetime. As
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from electronic stopping in ceramics and other insulating materials. In order to limit volatilization in any cement system tested, the particle flux should be kept below 1×1012 p/cm2-sec. This flux will limit significant volatilization from the cement. Fluxes greater than this can result in macroscopic failure as seen in the figures below. Using such low fluxes does make it difficult to (i) identify the irradiation area on the target and (ii) perform radiations that simulate long term exposure. Future experiments should use these parameters as starting points for performing irradiations. The investigators would like to acknowledge the outstanding support they received from Mr. Kim Kriewaldt at the University of Wisconsin’s Ion Figure 3. SEM image of irradiated A major finding of this study is Beam Laboratory. The experiments nanocement showing degree of that future experiments should subsurface cracking. required many on-the-fly changes be conducted in a differentially to the experimental end station and pumped vacuum station or through sample mounting configurations. Mr. a foil (barrier) that would allow the Kriewaldt was extremely resourceful in concrete to be irradiated at pressures accommodating and supplying fixtures closer to ambient. This may eliminate to make the investigation successful. water degassing in a high-vacuum environment that may affect the A challenge for future experiments results prior to the irradiation. will be performing irradiations and identifying the regions to be A second major finding is that irradiated; this may be on the order of concrete does experience significant a 0.05 mm2 area after the irradiation. volatilization of hydrous components The irradiation zone should be during the irradiation. The volatil- identified via scribing or some other ization may be exacerbated by the mechanism so that post-irradiation vacuum environment. The hydrous characterization can properly identify bonds are also more sensitive to low fluence irradiations. Not having ionizing radiation as compared to x and y control of the sample stage metal-metal or metal-oxygen bonds. limited the ability to perform This is analogous to damage resulting irradiations without opening the
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chamber to air. This, and not being Future Activities Figure 4. Mass Spectrum pre, during, able to identify the irradiated area, Future goals are to expand the and post irradiation using a Stanford Research Systems Residual gas prevented extensive mechanical capabilities of the chamber so analyzer. Irradiation begins at ~2 properties measurements. Cursory that multiple irradiations can be minutes and stops at ~4 minutes. micro-hardness measurements performed on a single target. Further An increase in the water signal is (Vickers) indicate that the investigation should examine changes observed during the irradiation. Beam current used is ~80 nA. irradiated areas may be harder than in the mechanical properties. the native microstructure.
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities University of Wisconsin Tandem Accelerator Ion Beam Collaborators University of Illinois John Popovics (co-principal investigator), Paramita Mondal (co-principal investigator) University of Tennessee Chris Wetteland (co-principal investigator), Kurt Sickafus (co-principal investigator) University of Wisconsin Jeff Terry (co-principal investigator) Oak Ridge Kevin Field (co-principal investigator) National Laboratory
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An Atom Probe Tomography Investigation of the Response of Oxide-dispersion Nanoclusters to Non-similar Friction Stir Welds Chad Parish – Oak Ridge National Laboratory – [email protected]
This work provides basic science information on the ability to weld high performance radiation tolerant alloys for advanced nuclear systems.
his work examined friction stir that retains the nanostructured features, welds that had been subjected specifically the nano-oxide clusters. Tto He or heavy-ion irradiation. However, it is not presently known Nanostructured ferritic alloys (NFAs) whether these nano-oxides retain the are strong candidates for Generation same radiation tolerance that makes IV fission systems, but welding of as-fabricated NFAs attractive from an NFAs is an immature technology. We engineering point of view. Therefore, used atom probe to study the effect of we chose to investigate the question of irradiation upon the nanostructures of the radiation response of the nano- the weld region. oxides in an NFA FSW. We performed heavy ion and helium ion irradiations Project Description on an NFA FSW zone at fission-relevant Our goal was to determine by temperatures. This project involved irradiation whether friction stir using atom probe at the Center for welding (FSW)-processed NFA was Advanced Energy Studies (CAES) to grossly similar or different from investigate the irradiated zones. irradiation of as-fabricated NFAs. This is important because, if the weld Accomplishments process should reduce the overall This work first accomplished the radiation tolerance of the material, production of the FSW structure and then NFAs might not be usable in irradiation using heavy ions and helium advanced Gen IV and fast reactor ions, both at Oak Ridge National systems. NFAs show strong potential Laboratory (ORNL). The co-principal for application to the core structures investigator, Phil Edmondson, then in fast reactors or other advanced carried the ion-irradiated samples nuclear energy systems. However, any to CAES and used the focused ion structure will require welding and beam and atom probe to examine the joining, and welding of NFAs is not different ion irradiated conditions. well developed. Traditional fusion We then transferred the data to ORNL, (liquid state) welding is unusable where data analysis and manuscript because the oxide nanostructures in the preparation is underway. NFA simply coarsen in the weld pool Future Activities and the material ceases to be an NFA. Future activities involve finalizing the As has been previously demonstrated, data analysis, preparing a manuscript, both by our group and other groups, and submitting the manuscript to a FSW of NFAs can produce a structure journal for peer reviewed publication.
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Figure 1. Atom probe map showing nanoclusters (green) in ion irradiated friction welded NFA 14YW.
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Idaho National Laboratory Joanna Taylor (principal investigator) Oak Ridge Chad Parish (principal investigator), National Laboratory Phil Edmondson (co-principal investigator)
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Characterization on the Bor-60 Neutron Irradiated Austenitic Stainless Steels and Cast Stainless Steel Yong Yang – University of Florida – yongyang@ufl.edu
Figure 1. Spinodal decomposition in the ferrite phases of CF3 Cast Stainless Steel irradiated to 5, 10, 20 and 40 dpa, respectively.
he work was planned to system- systematic study, at an atomic level, ically characterize the 316 SA on neutron irradiation effects in light Tand 304 SA stainless steels and water reactor (LWR) internal struc- CF-3 cast stainless steels irradiated to tural materials at LWR relevant condi- 45 dpa at 320°C in the Bor-60 reactor. tions. By correlating the microstruc- Both transmission electron microscopy ture study with selected mechanical and atom probe tomography were tests, this proposed research provides used to study the irradiated induced a fundamental understanding of the nano-sized features, including disloca- response of austenitic stainless steels, tion, phase separation, and precipi- cast stainless steel (welds) during the tates. The output from the execution designed 40-year reactor life, and, of proposed study fills the existing more relevantly, during the extended knowledge gap by providing a more life of 60 years and beyond.
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Figure 2. Spinodal decomposition Cr fluctuation wavelength vs. irradiation dose.
Project Description for ensuring the safe operation of The proposed study aims to provide nuclear power plants, particularly a more fundamental and advanced at such high anticipated dose. As knowledge of the irradiation nuclear power plants age and neutron response in austenitic stainless steel fluence increases, detrimental effects and cast stainless steel at LWR end- resulting from radiation damage and of-life (EOL) relevant conditions. To related degradation of the structural extend the service lifetime of LWRs integrity of core internal compo- beyond 60 years, the integrity of nents have become an increasingly reactor components and the perfor- important regulatory concern for mance of structural materials must the reactor license renewal. The be evaluated adequately. The antici- proposed research is well aligned pated neutron dose on LWR internal with the U.S. Department of Energy structural material can be 50 dpa or Office of Nuclear Energy’s (DOE-NE) above. The accurate assessment and Sustainability of LWRs program and prediction of materials performance evaluating the materials’ integrity is under anticipated operating condi- a key need for considering the life tions are of particular importance extension for the existing LWRs.
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Figure 3. Ni-Si-Mn clusters in the irradiated ferrite phase.
Overall, this project is the first reported study on the ferrite phase in a duplex stainless steel ever irradiated to such a high neutron irradiation dose. It shows that the microstructural changes may saturate at much higher dose than normally expected: 5 dpa at a LWR relevant condition.
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Accomplishments For the G-phase precipitates, a decrease Microstructural evolutions including in number density and an increase spinodal decomposition (SD) in mean size were observed with the (Figure 1) and G-phase precipitation increase of neutron irradiation dose were quantified using the atom from 5 to 40 dpa (Figure 3). Overall, probe tomography for the ferrite this project is the first reported study Atom Probe Tomography phase in a duplex structure cast on the ferrite phase in a duplex stainless steel irradiated to 5, 10, stainless steel ever irradiated to such 20, and 40 dpa, respectively. The a high neutron irradiation dose and characterization really SD wavelength was calculated using it shows that the microstructural the radial distribution function changes may saturate at a much provides an unprecedented (RDF) analysis and the amplitude higher dose than normally expected: was obtained from Cr-frequency 5 dpa at a LWR relevant condition. distribution. Both the SD wavelength insight into the chemical Future Activities and amplitude increases follow a The project is now completed. logarithmic curve and begin to evolution of materials saturate after 20 dpa (Figure 2). under irradiation.
Distributed Partnership at a Glance — Yong Yang, Associate Professor, NSUF and Partners Facilities and Capabilities Nuclear Engineering Program, Center for Advanced Microscopy and Characterization Suite Energy Studies University of Florida Collaborators Argonne National Yiren Chen (co-principal investigator), Laboratory University of Florida Yong Yang (principal investigator), Zhangbo Li (collaborator)
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STEM/EELS Study of Fission Product Transport in Neutron Irradiated TRISO Fuel Particles Haiming Wen – Idaho State University – [email protected]
Understanding of fission products in irradiated TRISO fuel particles will facilitate design and fabrication of TRISO particles with improved performance and expedite the development and deployment of high- temperature gas reactors.
ristructural isotropic (TRISO) is a potential worker safety concern coated fuel particles are due to plate out on the cooler Tdesigned for use as nuclear- metallic parts of the helium pressure fuel particles in high temperature boundary. This safety concern high- nuclear reactors. They are composed lights the importance of identifying
of a uranium oxide (UO2) or the metallic fission product transport uranium oxy carbide (UCO) fuel mechanisms of 110mAg through the kernel protected by a series of TRISO coating layers. ceramic coating layers that retain Project Description fission products. The ceramic TRISO The objectives of this project are to coatings are a finely tuned fission study the distribution, composition, product containment system, which and structure of fission products consist of, in the order of increased in neutron irradiated SiC layer of distance from the fuel kernel, a the TRISO particles, using electron porous carbon buffer layer, an inner microscopy including scanning trans- pyrolytic carbon (IPyC) layer, a SiC mission electron microscopy (STEM), layer, and an outer PyC (OPyC) energy dispersive x-ray spectroscopy layer. The SiC layer is the primary (EDS), electron energy loss spectros- fission product barrier of the TRISO copy (EELS), high-resolution transmis- particle and serves as the principal sion electron microscopy (HRTEM), structural layer as well. Release of and precession electron diffraction certain metallic fission products, e.g., (PED), in an effort to enhance the Ag and Pd, through intact TRISO understanding of distribution, coatings has been evident for decades composition, structure, and transport around the world, as well as in the mechanisms of fission products. In recent Advanced Gas Reactor (AGR)-1 the past 40 years, numerous studies, experiment at Idaho National including reactor experiments, out- Laboratory. The release of 110mAg of-pile experiments, and simulations, have been performed to investigate the
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Figure 1. (a) (b) TEM images of a fission product precipitate; (c) STEM image of the same fission-product precipitate where the line indicates EDS line scan and the square represents a reference area for drift correction during EDS line scan; (d) EDS line scan results corresponding to (c); (e) STEM image of the same fission-product precipitate where the orange rectangle indicates EDS mapping area and the yellow square represents a reference area for drift correction during EDS mapping; (f) Pd map corresponding to EDS mapping area in (e).
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Figure 2. (a) STEM image; (b) precession electron diffraction derived ASTAR map, where the fission product precipitate highlighted in (a) with a red spot is located at a grain boundary indicated by a black line (the black line is drawn during ASTAR data analysis across the grain boundary so that the characteristics of the grain boundary are obtained); (c) EELS spectrum corresponding to the precipitate highlighted in (a); (d) zero-loss peak of the EELS spectrum corresponding to the precipitate highlighted in (a).
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fission product transport behavior and fission products in the SiC layer of a mechanisms. Grain boundary (GB) TRISO particle, neutron-irradiated diffusion, neutron induced diffu- to 3.6 × 1021 n/cm2 fast fluence at sion, catalytic Pd assisted transport, 1040°C, utilizing electron microscopy and vapor-phase migration all have methods. STEM was used to investigate been suggested as possible governing distribution of fission products; EDS in The advanced electron transport mechanisms. The previous STEM was employed to obtain fission studies, however, have not been able product composition; information to reproduce the transport behavior on structure of fission products microscopy techniques of fission products and the mecha- was acquired using HRTEM; PED nisms remain poorly understood. This derived ASTAR was executed to study available at CAES provide project is anticipated to contribute characters of grain boundaries where to an enhanced understanding of fission products are located; attempts the mechanisms of fission product were made to measure charge states great tools for studying transport in the irradiated SiC layer of precipitates using EELS. The of TRISO particles. Thorough under- experiments and data analyses were structure and composition of standing of fission product transport conducted by Haiming Wen, and the mechanisms in the SiC layer will samples were from the Advanced improve fuel modeling and design, Microscopy and Microanalysis fission products in neutron and better SiC layers and TRISO Program that Isabella van Rooyen is coated particles can be designed to in charge of under the Advanced Gas enhance retention of fission products Reactor Program of DOE-NE. Both irradiated nuclear fuels. and reduce their release. Eventually, Wen and van Rooyen participated TRISO coated particles with improved in the design of the project. — Haiming Wen, performance can be fabricated and Accomplishments were made toward this advancement will expedite the the technical goals. In summary, a Research Assistant Professor qualifying and licensing processes for high density of nanoscale fission TRISO coated particles. Hence, this product precipitates was observed research is contributing to achieving in the SiC layer close to the SiC-IPyC the objectives of U.S. Department interface, most of which are rich of Energy Office of Nuclear Energy in Pd, while Ag was not identified. (DOE-NE) to develop the next genera- Some Pd-rich precipitates contain tion nuclear reactors, particularly high U. Precipitates tend to have complex temperature gas reactors. structure. Although a precipitate appears to have uniform contrast in Accomplishments STEM, it may exhibit non-uniform The technical goals of the research contrast in TEM/HRTEM, which may are to determine the distribution, be caused by composition variations composition, and structure of
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throughout the precipitate (as concentration throughout the precipi- indicated by EDS), and by variations tate. Note that Si and C concentrations in crystal structure, orientation, or are from the SiC matrix. dislocation density among different Figure 2 displays STEM, ASTAR, and parts of the precipitate (as suggested EELS results. The ASTAR results indicate by HRTEM). ASTAR results indicate that the precipitate highlighted in that the majority of precipitates are (a) is located at a random high-angle located at random high-angle grain grain boundary with a misorienta- boundaries. Significant challenges tion angle of 30 degrees. Note that were encountered during EELS study this precipitate is the same with the and no useful EELS results were one studied in Figure 1. Although obtained. The challenges were ascribed it is clear from EDS results that this to the fact that the TEM specimen precipitate is Pd-rich, no peak corre- was not thin enough. The TEM sponding to Pd is evident in the EELS specimen was prepared previously in spectrum (c); the only peak present the Electron Microscopy Laboratory in the EELS spectrum corresponds to (EML) and, due to the significant C (that comes from the SiC matrix). radioactivity, it could not be further From the zero-loss peak (d), the thick- thinned at the Center for Advanced ness of the precipitate is computed Energy Studies (CAES). In addition, as 0.54 electron mean free path, it could not be shipped back to EML which is too thick to get good EELS for further thinning due to the limit results. In order to obtain good EELS in time and budget for this Rapid signals, the thickness needs to be on Turnaround Experiment (RTE) project. the order of 0.1 to 0.2 electron mean Although the EELS study was not free path. Thickness measurements successful, the other data (STEM, EDS, were conducted using EELS at many TEM/HRTEM, and ASTAR) enabled different locations and it was found significant accomplishments toward that the TEM specimen is too thick for the technical goals, which rendered EELS study. this project successful. Figure 3 shows TEM, HRTEM, STEM, Figure 1 shows TEM and STEM images and EDS results on another fission of a fission product precipitate and EDS product precipitate. From the TEM line scan and mapping results. In TEM and HRTEM images, there is contrast images (a) and (b), there is contrast variation across the precipitate and it variation throughout the precipitate, appears that there are multiple layers although the precipitate appears to have in the precipitate in the thickness uniform contrast in STEM image (c). direction of the TEM specimen. From EDS line scan and mapping indicate the HRTEM images, it appears that that the precipitate is rich in Pd, the parts with different contrast in however, there is variation in the Pd the precipitate have the same crystal
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Figure 3. (a) TEM image of a fission-product precipitate; (b) (c) (d) high-resolution TEM images of the fission-product precipitate in (a), where the rectangular areas indicated in (b) are magnified in (c) and (d) respectively; (e) STEM image of the same fission-product precipitate; (f) EDS spectrum corresponding to the EDS point scan indicated in (e).
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structure, however, they may have by variations in Pd concentration and slightly different orientation and/ by slightly different orientation and/ or dislocation density. The contrast in or dislocation density. the precipitate in the STEM image is Future Activities uniform and EDS point-scan results This project is now complete. indicate that this precipitate is rich in Pd, with a U concentration. Publications [1.] Haiming Wen, Isabella J. van STEM, EDS, TEM, and HRTEM results Rooyen, “Advanced electron on another fission product precipitate microscopy study of fission are displayed in Figure 4. In the STEM products in a TRISO coated image, the precipitate has uniform particle neutron irradiated to contrast. The EDS results indicate that 3.6 × 1021 n/cm2 fast fluence the precipitate is rich in Pd. Note at 1040°C,” International that the Cu concentration is from the Conference on Nuclear Materials TEM grid. Multiple EDS point scans 2017, June 25-26, Paris, France, indicate that there are variations in Pd accepted. concentration across the precipitate. Similarly, in TEM and HRTEM images, [2.] Haiming Wen, Isabella J. van there are contrast variations among Rooyen, “Distribution, composi- different parts of the precipitate. tion and structure of fission prod- From HRTEM images, the precipitate ucts in a TRISO coated particle appears to have a face centered cubic neutron irradiated to 3.6 × 1021 structure and different parts of the n/cm2 fast fluence at 1040°C,” precipitate have the same structure. journal paper in preparation The contrast variations may be caused
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Idaho National Laboratory Isabella J van Rooyen (co-principal investigator) Idaho State University Haiming Wen (principal investigator)
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Figure 4. (a) STEM image of a fission- product precipitate where the red circle indicates the position for a EDS point scan; (b) EDS spectrum corresponding to the EDS point scan indicated in (a); (c) TEM image of the same fission-product precipitate shown in (a); (d) (e) (f) high-resolution TEM images of the precipitate indicated in (c), where the rectangles in (d) are magnified in (e) and (f), respectively.
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Investigation of Dislocation Loop Hardening and Stability in Irradiated RPV Steels Peter Wells – University of California, Santa Barbara – [email protected]
Figure 1. Atom probe maps from ne potential barrier to Safely extending the lifetime of the the Ni-free steel (LA) showing extending light water reactor US fleet of LWRs will require robust evolution of both CRP and (LWR) lifetimes to 80 years is prediction models that not only include dislocation loop enrichment O under annealing. embrittlement of their massive reactor the effect of irradiation variables such pressure vessels (RPV). Embrittlement as neutron flux, fluence, and operating is primarily due to the formation of temperature, but also alloy chemistry. nm-scale precipitates as well as solute This research aims to better understand defect clusters, which cause hardening the role of alloy Ni content in the and a corresponding increase in the formation and thermal stability of hard- ductile-to-brittle transition temperature. ening features formed under irradiation.
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The insight gained from atom probe tomography on this series of irradiated alloys will enable us to make better, physically based predictive models for extended life LWR operation. Annealing and atom probe tomography characterization Project Description temperatures up to 500°C. Thus, the A recent Nuclear Science User purpose of this experiment was to of these RPV steels provides Facilities (NSUF) funded irradiation use APT and transmission electron in the Advanced Test Reactor included microscopy (TEM) to investigate four reactor pressure vessel steels with the microstructure of both the a quantitative assessment of the same nominal bulk Cu contents as-irradiated and the irradiated and (Д0.4 wt.%) but varying Ni levels annealed low Ni alloys to better the various hardening features (0.01, 0.18, 0.84, and 1.25 wt.%) measure both the precipitates and the to isolate this element’s effect on dislocation loops. irradiation hardening. The samples formed under irradiation, Accomplishments were irradiated to 1.7 dpa at Д 310°C. Atom probe tomography and Microhardness on the irradiated transmission electron microscopy supporting model development samples showed that the steels with were both completed on the two low lower Ni contents (0.01-0.18) had Ni steels. The atom probe showed much less hardening than those with at extended life LWR fluences. large dislocation loops (
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Figure 2. Line profiles through seen in Figure 2, show enrichment anneal, seen in both Figures 1 and 2, dislocation loops showing change of Mn on the outer edges of the loop but some slight Mn segregation was in solute segregation around dislocation loops under annealing. and Si enrichment on the inner edges. still observed. After the 500°C anneal, Sequential post irradiation annealing the loops were only slightly enriched treatments for 1 week each were in Mn, but also significantly enriched performed at temperatures between in Mo and C. These results will be 350°C and 550°C in 25°C increments used to better calibrate hardening in order to track the changes in both models and determine the hardening the Cu-rich precipitates and also the efficiency of dislocation loops and solute segregation to dislocation loops. precipitates. In addition, they can help The precipitates in the 450°C and to better understand radiation induced 500°C annealed samples, also shown segregation of various elements. in Figure 1, began coarsening but Future Activities still had slight Mn enrichments. The This work is part of a much larger Si was no longer enriched around project designed to create an RPV the dislocation loops after the 450°C embrittlement prediction model for extended life fluences. These results
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have helped to guide the creation of [2.] P. B. Wells, N. Almirall, G. R. this model, but future work will focus Odette, T. Yamamoto, D. Gragg, H. on generating a large database of high Ke, D. Morgan, “Thermal stabil- fluence embrittlement for various RPV ity of hardening features formed alloys and irradiation conditions. under high dose neutron irradia- tion,” International Group of Publications Radiation Damage Mechanisms [1.] P. B. Wells, N. Almirall, G. R. 19th Semiannual Meeting, Asheville, NC Odette, T. Yamamoto, D. Gragg, April 10-15, 2016. H. Ke, D. Morgan, “Thermal Stability of Nanoscale Mn-Ni-Si A publication of this study is planned. Precipitates in Irradiated Reactor Pressure Vessel Steels,” TMS 2016 Annual Meeting, Nashville, TN, February 15-19, 2016.
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, Hot Fuel Examination Facility Collaborators University of California, G. Robert Odette (co-principal investigator), Santa Barbara Takuya Yamamoto (co-principal investigator), Peter Wells (co-principal investigator), Nathan Almirall (collaborator)
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Microstructure Characterization of High-energy Xe Ion Irradiated U-Mo Bei Ye – Argonne National Laboratory – [email protected]
Figure 1. An overview of the TEM sample prepared from a U-Mo/Al sample irradiated with 84 MeV Xe ions to a dose of 2.9 × 1017 ions/cm2.
The information obtained in this study provides new perspective on microstructural evolution in nuclear fuels under irradiation, for example, irradiation induced recrystallization.
n this project, U-Mo/Al dispersion Project Description fuel samples irradiated with high U-Mo/Al dispersion fuels, developed Ienergy heavy ions were character- for reducing uranium enrichment ized with TEM to reveal ion modified in research and test reactor fuels for microstructure in U-Mo. Qualitative non-proliferation purpose, underwent and quantitative assessments of the drastic microstructural changes microstructural evolution of U-Mo during in-pile irradiations, including as a function of the ion penetration the excessive growth of (U,Mo)AlX depth were obtained. interdiffusion layer and large fission gas filled pores at the interfaces of U-Mo fuel particles and the Al matrix.
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The characterization experiments at CAES revealed a lot of new information of the microstructure of irradiated
Figure 2. The magnified view of the “A1” area marked in Figure 1, showing the U-Mo fuel. microstructure of the (U,Mo)Alx layer. These microstructural changes degrade Al dispersion fuels. By comparing — Bei Ye, fuel thermal conductivity, increase the post-irradiation examination Materials Scientist fuel temperature, and eventually lead (PIE) results of carefully selected to excessive fuel swelling. In order samples, a qualitative assessment of to improve the fuel’s irradiation the effects of dose, dose rate, U-Mo performance, it is critical to adjust grain size, irradiation temperature, fuel fabrication parameters based and Mo contents on U-Mo/Al on the correct understanding of the irradiation behavior can be obtained. causes of the microstructural changes. The characterization results of ion Heavy ion irradiation was employed irradiated fuels will be used in to screen fuel fabrication variables designing the next irradiation test and to investigate separate effects in reactor. of irradiation behavior of U-Mo/
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a) b)
Figure 3. The magnified views of Accomplishments Future Activities the “A2” area marked in Figure 1 TEM specimens of irradiated U-Mo/Al The TEM study performed in 2016 taken at the (a) underfocus and (b) overfocus conditions, showing the dispersion fuel were fabricated using revealed the microstructure of heavy high density nano-bubbles inside the FEI Quanta focused ion beam (FIB) ion irradiated U-Mo at certain fuel grains. and characterized at the Tecnai STEM irradiation temperature and dose at the MaCS at CAES. Several 20 × 20 rate. We will expand the investigation × 10 μm3 U-Mo cubes were lifted out to samples irradiated at different using the FEI Quanta FIB for synchro- temperatures and dose rates. tron irradiation characterization at the Publications APS MRCAT Line at Argonne National [1.] B. Ye, L. Jamison, S. Bhattacharya, Laboratory. Additional TEM specimens A. Yacout, “TEM Characterization were prepared from un-irradiated of U-Mo Irradiated with High- U-Mo fuel using the FIB for in-situ Energy Xe Ions,” Transaction of irradiation study at the IVEM Facility ANS Nuclear Society 114, (2016) at ANL. All FIB prepared samples were 1285–1288. readied by the team with the great help of Jatu Burns. Joanna Taylor helped a great deal in shipping and handling the radioactive samples.
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Figure 4. The magnified view of the “A3” area marked in Figure 1, showing second-phase precipitates forming beyond the Xe deposition range.
Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Argonne National Bei Ye (principal investigator), Laboratory Laura Jamison (collaborator), Yinbin Miao (collaborator)
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Effects of Carbon Addition on Solute Redistribution in Fe-9Cr Alloys Under Irradiation Cheng Sun – Oak Ridge National Laboratory /Idaho National Laboratory – [email protected]
Figure 1. EBSD mapping he designs of the next genera- Project Description showing the į-ferrite phase in tion of nuclear reactors call for Fe-9Cr alloys are leading candidates an equiaxed morphology and the development of materials for cladding and core components in tempered martensite phase in a T lath structure. The portion of high- that can withstand severe neutron the next generation of nuclear reactors. angle grain boundaries in this irradiation over a wide range of Two issues that limit their lifetime Fe-9Cr alloy is 77.5%. temperatures. Fe-Cr-based alloys at high doses are hardening at low are leading candidates for cladding temperatures and doses, and void and core structure applications in swelling at high doses and intermediate reactors. Radiation induced solute temperatures. A fundamental redistribution results in the degrada- understanding of the effects of carbon tion of mechanical properties and in these alloys will aid in overcoming structure integrity. This research these obstacles. Surveys of irradiation focused on the microstructure and behavior of alloys by neutron and ion microchemistry characterization of irradiation indicate that the nucleation high dose irradiated Fe-Cr alloy by and growth kinetics of radiation advanced electron microscopy and induced defects are strongly influenced atom probe tomography. by the minor elemental additions. The hypothesis is that carbon vacancies can trap small dislocation loops and prevent
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Figure 2. Atom probe tomography of tempered martensite in as- A fundamental understanding of the effects of carbon on the received Fe-9Cr alloy. Enrichment solute redistribution in these alloys will help us design the of carbon and titanium in the grain chemical composition of Fe-Cr based alloys with improved boundary were obtained. radiation performance in nuclear reactors. a migration towards sinks. At the same Accomplishments time, vacancies are inclined to diffuse We have prepared Fe-9Cr with to voids and promote the growth of 0.02wt.% C samples for irradiation voids at intermediate temperatures. studies. High temperature and high The impact of carbon addition on the dose irradiation experiments were accumulation of defect clusters and performed in the Michigan Ion solute redistribution in Fe-9Cr alloys Beam Laboratory at the University of during ion irradiation is not clear. Michigan. By using electron back- This research provided fundamental scatter diffraction (EBSD), we identi- knowledge on the materials fied two phases in the matrix: they degradation of materials in reactor are ĝ-ferrite and tempered martensite. environments and sheds light on the Atom probe tomography at the Center design of microstructure in radiation for Advanced Energy Studies (CAES) resistant materials for advanced nuclear was used to measure the differences reactors of many types, including light in chemistry in both phases. The water cooled reactors. focused ion beam at the CAES was utilized to make samples for atom probe tomography (APT) analysis and TEM characterization. The results
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Figure 3. Bright-field and dark- field TEM micrographs of irradiated ĝ-ferrite in Fe-9Cr alloy. Irradiation-induced voids were formed in the damaged region.
indicate that carbon concentration in MIBL, University of Michigan, tempered martensite is lower than that Gary Was. in -ferrite phase and TEM micro- ĝ IVEM, Argonne National Laboratory, graphs of irradiated samples suggest Mark Kirk. that tempered martensite exhibits a stronger swelling resistance. This SCK CEN, Belgian Nuclear might be attributed to the lowered Research Centre, L. Malerba and carbon concentration in tempered M. Konstantinovic. martensite and/or sink effects of lath Future Activities boundaries. In addition, we performed A new proposal based on this research in-situ irradiation experiments at the has been submitted to NSUF. Intermediate Voltage Electron Micros- copy (IVEM) Facility at Argonne Publications National Laboratory to understand [1.] C. Sun, et al., “Void swelling of the influence of carbon addition on ĝ-ferrite and tempered martensite the growth kinetics of dislocation in a Fe-9Cr model alloy subjected loops at 300°C. This research provided to 8 MeV Fe ion irradiation,” 2017 a comprehensive understanding on Environmental Degradation of Materials in how carbon addition affects the solute Nuclear Power Systems—Water Reactors redistribution of Fe-9Cr alloy under Conference, submitted. irradiation at different conditions. We would like to acknowledge the following institute and individuals for the contribution.
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MaCS at CAES facility has provided opportunities to
Figure 4. Bright-field and dark-field TEM micrographs of irradiated tempered perform world-class research martensite phase in Fe-9Cr alloy. Irradiation-induced voids were formed in the damaged region. The void density is much lower compared to that in irradiated ĝ-ferrite phase. on nuclear materials.
— Cheng Sun, Postdoc Distributed Partnership at a Glance NSUF and Partners Facilities and Capabilities Center for Advanced Microscopy and Characterization Suite Energy Studies Collaborators Argonne National Stuart Maloy (co-principal investigator) Laboratory Idaho National Assel Aitkaliyeva (co-principal investigator) Laboratory
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NSUF LIST OF ACRONYMS
AGR ...... Advanced Gas Reactor ANL ...... Argonne National Laboratory ANS ...... American Nuclear Society APT ...... Atom Probe Tomography ASR ...... Alkali-Silica Reaction ATLAS ...... Argonne Tandem Linac Accelerator ATR ...... Advanced Test Reactor BNL ...... Brookhaven National Laboratory BR-2 ...... Belgium Reactor-2 CAES ...... Center for Advanced Energy Studies CINR ...... Consolidated Innovation in Nuclear Research CRSS ...... Critical Resolved Shear Stress DOE ...... U.S. Department of Energy DOE-NE ...... U.S. Department of Energy Office of Nuclear Energy dpa ...... Displacements Per Atom EBSD ...... Electron Backscatter Diffraction EDS ...... Energy Dispersive X-Ray Spectroscopy EELS ...... Electron Energy Loss Spectroscopy EML ...... Electron Microscopy Laboratory EOL ...... End-of-Life EPRI ...... Electric Power Research Institute F/M ...... Ferritic/Martensitic FIB ...... Focused Ion Beam FOA ...... Funding Opportunity Announcement FSW ...... Friction Stir Welding FY ...... Fiscal Year GAIN ...... Gateway for Accelerated Innovation in Nuclear
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GB ...... Grain Boundary HFEF ...... Hot Fuels Examination Facility HIP ...... Hot Isostatic Pressing HQ ...... Headquarters HRTEM ...... High-Resolution Transmission Electron Microscopy HTTL ...... High Temperature Test Laboratory IFP ...... Inverse Pole Figure IML ...... Irradiated Materials Laboratory INL ...... Idaho National Laboratory IVAS ...... Interactive Analysis and Visualization Software IVEM ...... Intermediate Voltage Electron Microscopy IXB ...... Ion X-Ray Beam LEAP ...... Localized Electron Atom Probe LWR ...... Light Water Reactor MA ...... Mechanical Alloying MaCS ...... Microscopy and Characterization Suite MFC ...... Materials and Fuels Complex MIT ...... Massachusetts Institute of Technology MRCAT ...... Materials Research Collaborative Access Team MRS ...... Materials Research Society NEET ...... Nuclear Energy Enabling Technology NEID ...... Nuclear Energy Infrastructure Database NFA ...... Nanostructured Ferritic Alloy NFML ...... Nuclear Fuels and Materials Library NFS ...... Nanostructured Ferritic Steels NSLS-II ...... National Synchrotron Light Source II NSUF ...... Nuclear Science User Facilities NuMat ...... Nuclear Materials Conference ODS ...... Oxide-Dispersion-Strengthened ORNL ...... Oak Ridge National Laboratory PED ...... Precession Electron Diffraction PI ...... Principal Investigator PIE ...... Post-Irradiation Examination
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PNNL ...... Pacific Northwest National Laboratory RDF...... Radial Distribution Function RFI ...... Request for Information RIS ...... Radiation-Induced Segregation RPV ...... Reactor Pressure Vessel RTE ...... Rapid Turnaround Experiment SAM ...... Sample Library SD ...... Spinol Decomposition SEM ...... Scanning Electron Microscope SPS ...... Spark Plasma Sintering STEM ...... Scanning Transmission Electron Microscopy TEM ...... Transmission Electronic Microscope TMS ...... The Minerals, Metals and Materials Society TREAT ...... Transient Reactor Test TRISO...... Tristructural Isotropic TRL ...... Technology Readiness Level XMAT ...... Extreme Materials Beam Line
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NSUF INDEX
NSUF & Partners/ Idaho National Laboratory: Hot Fuel Purdue University: 25, 30, 33, 43, 44, 56 Examination Facility (HFEF), 39, 45, 85, 96 Facilities & Capabilities Texas A & M University: 43, 45, 60, Argonne National Laboratory: 30, 36, Idaho National Laboratory: Irradiation- 62, 63 37, 43, 44, 45, 73, 86, 88, 89, 92, 93, 95 Assisted Stress Corrosion Cracking Facility, 19 University of California, Berkeley: 30, Argonne National Laboratory: Idaho National Laboratory: Materials and 44, 45, 48, 50, 53 Intermediate Voltage Electron Microscopy Fuels Complex (MFC), 2, 4, 8, 14, 20, 33, 39, (IVEM)-Tandem Facility, 36, 39, 43 University of California, Berkeley: 45, 48, 50, 53, 96 Nuclear Materials Laboratory, 50, 53 Brookhaven National Laboratory: 8, 43 Idaho National Laboratory: Colorado School of Mines: 21, 33, 45 Brookhaven National Laboratory: Transient Reactor Test Facility (TREAT), 8 National Synchrotron Light Source II, 8 University of Florida: 26, 29, 33, 45, Idaho State University: 21, 33, 43, 45, 70, 73 Canadian Nuclear Laboratories, 53, 95 74, 80 University of Idaho: 18, 22, 45, 60, 63 Center for Advanced Energy Studies Illinois Institute of Technology: 30, 33, (CAES): 6, 18, 22, 25, 30, 33, 44, 54, 55, 44, 45, 96 University of Illinois: 45, 67 57, 58, 59, 60, 62, 63, 68, 69, 73, 77, 78, Los Alamos National Laboratory: 21, University of Michigan: 30, 92 80, 85, 87, 88, 89, 91, 93, 95 43, 45, 54, 55 University of Michigan: Center for Advanced Energy Studies Massachusetts Institute of Technology: Michigan Ion Beam Laboratory, 33, 41, 42, 43, (CAES):Microscopy and Characterization Suite 30, 43, 44, 96 59, 91 (MaCS), 6, 23, 24, 25, 28, 55, 57, 60, 62, 63, 88, 93, 96 Massachusetts Institute of Technology: University of Nevada Las Vegas: 16, 30, MIT Nuclear Materials Laboratory, 43 44, 45 Electric Power Research Institute: 8, 40 North Carolina State University: 30, 44, University of Tennessee: 43, 45, 64, GE Hitachi Nuclear Energy: 33, 45 45, 96 65, 67 Idaho National Laboratory: 2, 4, 8, 9, Oak Ridge National Laboratory: 30, 33, University of Wisconsin: 26, 30, 43, 44, 14, 19, 20, 25, 26, 27, 30, 33, 39, 44, 45, 44, 45, 67, 68, 69, 90, 97 66, 67 47, 53, 59, 69, 74, 80, 85, 90, 93, 96 Oak Ridge National Laboratory: University of Wisconsin: Idaho National Laboratory: High Flux Isotope Reactor (HFIR), 33, 96 Tandem Accelerator Ion Beam, 33, 67 Advanced Test Reactor (ATR), 7, 8, 11, 12, 25, 26, 29, 33, 38, 47, 56, 59, 83, 85, 95 Oak Ridge National Laboratory: Low Vanderbilt University, 33 Activation Materials Design and Analysis Idaho National Laboratory: Westinghouse: 30, 33, 44 Laboratory (LAMDA), 33, 96 Analytical Laboratory, 2 Westinghouse: Materials Center of Oak Ridge National Laboratory: ORNL Idaho National Laboratory: Excellence Laboratories (MCOE) Hot Cell Gamma Irradiation Facility, 33 Electron Microscopy Laboratory, 53, 78, 95 Facility, 30 Oregon State University: 22, 33, 45 Idaho National Laboratory: Electron Microscopy Laboratory, 53, 78, 95 Pacific Northwest National Laboratory: 15, 30, 45
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Analytical Laboratory, MFC, INL
Collaborators Field, Kevin Li, Zhangbo Aitkaliyeva, Assel Oak Ridge National Laboratory 67, 99 University of Florida 73 Idaho National Laboratory 93, 99 Griffiths, Malcolm Maloy, Stuart Almirall, Nathan Queen’s University 53, 99 Argonne National Laboratory 93 University of California, Santa Barbara 83, Guria, Ankan Miao, Yinbin 85, 99 University of Idaho 63 Team Member – Student Argonne National Laboratory 89, 100 Burns, Jatuporn 62, 63 Mondal, Paramita Boise State University 59, 62, 63, 88, 99 Hackenberg, Robert University of Illinois 67 Charit, Indrajit Los Alamos National Laboratory 55 Odette, G. Robert University of Idaho 60, 63 Hosemann, Peter University of California, Santa Barbara 85, 100 Chen, Yiren University of California, Berkeley 48, 53 Parish, Chad Argonne National Laboratory 73, 99 Howard, Cameron Oak Ridge National Laboratory 68, 69 Clarke, Amy University of California, Berkeley 50, 53 Parker, Steven Scott Los Alamos National Laboratory 55 Jamison, Laura University of California, Berkeley 50, 53 Dolph, Corey K. Argonne National Laboratory 88, 89, 99 Pasebani, Somayeh Boise State University 58, 59, 99 Judge, Colin University of Idaho Team Member – Student Edmondson, Phil Canadian Nuclear Laboratories. 50, 53, 100 62, 63 Oak Ridge National Laboratory 33, 68, 69
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Popovics, John Wetteland, Chris University of Illinois 67 University of Tennessee 64, 65, 67 Shao, Lin Wharry, Janelle Texas A&M University 60, 62, 63 Boise State University 22, 25, 33, 56, 58, 59, 100 Sickafus, Kurt University of Tennessee 67 Wu, Yaqiao Boise State University 58, 62, 63, 100 Swenson, Matthew Boise State University 22, 23, 25, 58, 59, 100 Xu, Steven Kinectrics Inc. 53 Taylor, Joanna Idaho National Laboratory 58, 62, 69, 88, 100 Yablinsky, Clarissa Los Alamos National Laboratory 54, 55 Terry, Jeff University of Wisconsin 67, 100 Yamamoto, Takuya University of California, Santa Barbara 85, 100 van Rooyen, Isabella J Idaho National Laboratory 77, 80, 100 Yang, Yong University of Florida 26, 27, 29, 33, 70, Wells, Peter 73, 100 University of California, Santa Barbara 82, 85, 100 Ye, Bei Argonne National Laboratory 86, 87, 89 Wen, Haiming Idaho State University 33, 74, 77, 80
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Irradiated Materials Characterization Laboratory (IMCL), MFC, INL101 // NldN! ~ OSm FdllM Nuclear Science 995 Urwetlllf)' Bclclltw:lra User Facilities ldallo ,_...._JO BJ;t01 SSM c @il.SUr www.mutlinl p J 17-50050-R16