Methods, Techniques, and Materials Discovery of Irradiation Effect Using In-situ Microscopy: Applications of X-ray/Neutron Diffraction and Imaging Techniques
Sponsored by: TMS Structural Materials Division, TMS: Nuclear Materials Committee, TMS: Advanced Characterization, Testing, and Simulation Committee
Program Organizers: Wei-Ying Chen, Argonne National Laboratory; Xuan Zhang, Argonne National Laboratory; Kevin Field, University of Michigan; Donald Brown, Los Alamos National Laboratory; Aida Amroussia, GE Global Research
Tuesday 2:30 PM
March 21, 2023
Room: 25A
Location: SDCC
Session Chair: Xuan Zhang, Argonne National Laboratory
2:30 PM Invited
Perspectives on Quasi-in-situ Characterization of Nuclear Materials Using Synchrotron X-rays: Maria Okuniewski1; Alejandro Figueroa Bengoa1; Sri Tapaswi Nori2; Peter Kenesei3; Jun-Sang Park3; Jonathan Almer3; 1Purdue University; 2NOMATEN Centre of Excellence; 3Argonne National Laboratory
In-situ characterization of the microstructure of materials while conducting neutron irradiations is extremely challenging due to the harsh environments within nuclear reactors. However, quasi-in-situ microstructural characterization can be carried out on nuclear materials by non-destructively examining the same specimen prior to and after neutron irradiation. Although this technique does not capture dynamic events that occur during irradiation, it does enable a more comprehensive understanding of neutron damage to a specific microstructure. This talk will focus on the use of synchrotron imaging and diffraction techniques applied to a neutron irradiated structural material.
3:00 PM Invited
Revealing 3D Microstructures in Nuclear Materials with High-energy X-rays: Jonathan Almer1; Peter Kenesei1; Jun-Sang Park1; Hemant Sharma1; Xuan Zhang1; Meimei Li1; 1Argonne National Laboratory
High-energy x-rays from 3rd generation synchrotron sources, including the Advanced Photon Source (APS), possess high penetration power and high spatial, reciprocal space, and temporal resolution. These characteristics enable 3D imaging using both density and scattering contrast. Within the X-ray Science Division at the APS, we have developed 3D techniques to study polycrystalline materials through (i) absorption-based tomography, (ii) high-energy diffraction microscopy (HEDM or 3DXRD) and (iii) scattering tomography. HEDM provides diffraction information (strain, orientation, shape and size) of individual grains in aggregates while complementary scattering tomography provides spatially resolved but grain-averaged information. Use of these techniques for both ex situ and in situ studies of nuclear-relevant materials will be presented, along with descriptions of enabling in situ equipment. Further developments will be discussed in the context of the imminent APS upgrade, which will include a new high-energy x-ray beamline and Activated Materials Laboratory on the APS premises.
3:30 PM
In-situ 3D High-energy X-ray Diffraction Study on Deformation Behavior of Neutron-irradiated Fe-9%Cr: Dominic Piedmont1; Jun-Sang Park2; Peter Kenesei2; Jonathon Almer2; Matthew Kasemer3; Ezra Mengiste3; James Stubbins1; Meimei Li2; Xuan Zhang2; 1University Of Illinois At Urbana-Champaign; 2Argonne National Laboratory; 3University of Alabama
Given the extreme environments nuclear reactor core structural materials are exposed to, significant effort must be made to understand the microstructure-property correlation. However, there is a discontinuity of length scales under common investigation of materials. Mechanical testing provides insight to bulk behavior while electron microscopy gives nano- to micro-meter scale information. Presented is a direct link between the discontinuous length scales previously observed, via grain scale (meso-scale) characterization of deformation responses in irradiated materials. Using synchrotron x-rays, high energy x-ray diffraction microscopy (HEDM) nondestructively probes mm-size samples to obtain grain-resolved information in-situ and ex-situ. The resulting data allows for observations of grain rotation and residual strain evolutions as a function of deformation. Results were obtained for Fe-9%Cr samples: two irradiated to 0.1 dpa at temperatures of 300°C and 450°C, and one unirradiated sample for comparison. Experimental results are compared to computational results from Crystal Plasticity Finite Element Modeling (CPFEM) simulations.
3:50 PM Break
4:10 PM Invited
Quantifying the Recovery of Irradiated and Cold-worked Zr-2.5Nb Using X-ray and Neutron Diffraction Line Profile Analysis: Levente Balogh1; Thalles Lucas1; Fei Long1; Aaron Barry2; Mark Daymond1; Donald Brown3; 1Queen's University; 2Royal Military College of Canada; 3Los Alamos National Laboratory
Recovery kinetics of dislocation structures formed by either cold-work or irradiation are expected to be different due to the dissimilar configuration of lattice dislocations and dislocation loops. Zr-2.5Nb pressure tube (PT) material was irradiated by fast neutrons at 250 deg C which induced dislocation loops, and unirradiated Zr-2.5Nb PT samples were plastically deformed at 250 deg C to introduce a high density of cold-work dislocations. Samples from the irradiated material were in-situ annealed isothermally and measured using neutron diffraction, while the cold-worked samples were annealed isothermally and characterized ex-situ using high resolution synchrotron X-ray diffraction. The diffraction patterns were evaluated by Diffraction Line Profile Analysis (DLPA) to quantitatively characterize the dislocation density and character as a function of annealing time and temperature. The activation energy and the pre-exponential factor of the recovery process was obtained for both the irradiation-induced and cold-work dislocations, and their differences will be discussed in detail.
4:40 PM
Revealing Heat-treatment Induced Stoichiometric Variations in Neutron-irradiated
Yttrium Hydrides Using In Situ Synchrotron Radiation Diffraction: Mahmut Cinbiz1; Mehmet Topsakal2; Annabelle Le Coq3; Kory Linton3; 1INL; 2Brookhaven National Laboratory; 3Oak Ridge National Laboratory
Neutron-irradiated and fresh yttrium hydride specimens were characterized in situ using high-energy synchrotron x-ray diffraction experiments while the samples were subjected to heat treatments. The evolution of the yttrium hydride and minor yttrium phases were monitored as a function of temperature and time. The high-energy synchrotron x-rays enabled to determine hydrogen redistribution in the samples during the heat treatments. While heating, the initial yttrium phase completely dissolved above 400˚C in all samples. During the cooling stage of the fresh sample, the initial yttrium phase re-appeared around 200˚C, but its intensity was lower than its initial intensity. For irradiated samples, yttrium phase unexpectedly diminished during the cooling stage, which revealed a positive shift on the hydrogen atomic fraction after heat treatments while expecting vice versa. This indicated that yttrium hydride superior phase stability. Observations were speculated by the release of trapped hydrogen from pre-existing and irradiation-induced defects
5:00 PM
Laboratory-based 3D X-ray Imaging of Neutron-irradiated TRISO Fuel: Nikolaus Cordes1; Brian Gross2; William Chuirazzi2; Rahul Kancharla2; Fei Xu2; Joshua Kane2; John Stempien2; 1Los Alamos National Laboratory; 2Idaho National Laboratory
Micro X-ray computed tomography (micro-XCT) has been used to image neutron-irradiated tristructural isotropic (TRISO) coated fuel particles and compacts at Idaho National Laboratory’s (INL) Irradiated Materials Characterization Laboratory. This presentation will give an overview of the 3D imaging, accomplished with a laboratory-based X-ray microscope (a ZEISS Xradia 520 Versa). Compacts were irradiated in INL’s Advanced Test Reactor as part of the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program. Individual particles are from compacts irradiated during the second series of tests (i.e., AGR-2) and TRISO compacts are from the combined third and fourth series of tests (i.e., AGR-3/4). This work was sponsored by the U.S. Department of Energy, Office of Nuclear Energy, through the Advanced Reactor Technologies Advanced Gas Reactor Fuel Development and Qualification Program. Idaho National Laboratory is operated by Battelle Energy Alliance LLC under contract number DE-AC07-05ID14517 for the U.S. Department of Energy.