Neutron and X-ray Scattering in Materials Science: Micro to Meso Scale Structure
Sponsored by: TMS Functional Materials Division, TMS: Chemistry and Physics of Materials Committee
Program Organizers: Michael Manley, Oak Ridge National Laboratory; Chen Li, University of California-Riverside; Jennifer Niedziela, Oak Ridge National Lab; Hillary Smith, Swarthmore College
Wednesday 2:00 PM
March 22, 2023
Room: Aqua 311B
Location: Hilton
Session Chair: Raphael Hermann, Oak Ridge National Laboratory
2:00 PM
Effect of Deformation on Microstructure Evolution In Dilute MgYZn Alloys Examined by Combined Use of SWAXS and EXAFS: Hiroshi Okuda1; Yoshiaki Maegawa1; Yoshihito Kawamura2; Shin-ichi Inoue2; 1Kyoto University; 2Kumamoto University
Dilute Mg-Y-Zn alloys containing partial structure of long-range stacking ordered (LPSO) phase attracted attention due to their capability of kink deformation upon deformation. The microstructures and their evolution in those alloys were examined by in-situ small- and wide angle X-ray scattering and EXAFS at the Zn K absorption edge. In the early stage of precipitation, in-situ SWAXS suggests development of very thin two-dimensional segregation layer of clusters at elevated temperatures, while deformation at elevated temperatures gives thicker segregation layers. Since the dilute alloys of engineering interest consist of fine-grained polycrystalls, the SAXS pattern gave a specific fog-box like profiles. The effect of deformation on the microstructural evolution was examined by comparing the temporal developments of the two conditions. The clusters in the segregation layers was also examined by EXAFS at the Zn absorption edge.
2:20 PM Cancelled
In-situ High-resolution X-ray Nanotomography of the Thermal Sintering and Densification of a Chlorine Bearing Vanadinite Apatite Nuclear Waste Form: Joshua Kane1; Jorgen Rufner1; Tiankai Yao1; William Chuirazzi1; Rahul Kancharla1; Xianghui Xiao2; Dong Zhao3; Jie Lian3; 1Idaho National Laboratory; 2Brookhaven National Laboratory; 3Rensselaer Polytechnic Institute
Chlorine-36 (36Cl) is a fission product representing a significant challenge to fuel pryoprocessing and storage. Traditional borosilicate waste forms poorly immoblize 36Cl and chlorine incorporation within silicates reduces the desired properties. Vanadinite apatite, Pb5(VO4)3X, has been proposed as an alternative to a borosilicates as it strongly immobilizes 36Cl and possess good stability and mechanical properties. Its sintering, however, can be challenging due to potential Cl loss at elevated temperatures. Here, the densification of high energy ball milled Pb5(VO4)3Cl powder via thermal sintering is examined in-situ with X-ray nanotomography at the FXI beamline at the NSLS-II. Tomographic scans were collected on individual particle agglomerates heated, in a custom FXI beamline furnace, to sintering temperatures and tracked throughout their densification. 3D correlation, post-processing, and analysis of tomographic data during sintering will be presented and utilized to provide insight into the sintering and evolution of Pb5(VO4)3Cl for nuclear waste forms for 36Cl.
2:40 PM
Irradiated Graphite Across Microscopic to Mesoscopic Length-scales: Boris Khaykovich1; David Sprouster2; Anne Campbell3; Durgesh Rai4; Jan Ilavsky5; Lance Snead2; 1Massachusetts Institute of Technology; 2Stony Brook University; 3Oak Ridge National Laboratory; 4Xenocs Inc; 5Argonne National Laboratory
Graphite is a fascinating material that has been prominent in nuclear reactors since the days of the Chicago Pile until today. When irradiated, graphite undergoes initial densification (or shrinkage) by as much as 10%, followed by swelling. The amount of radiation damage at which the swelled graphite’s volume equals that before irradiation determines the end of life of graphite parts and in some cases the life of the reactors themselves. This parameter has to be painstakingly measured for each new graphite type and each new irradiation condition. Given graphite’s enormous complexity and variability, reliable prediction of the irradiation response by molecular-dynamic simulations has not yet been possible. We used synchrotron SAXS and WAXS techniques to uncover the connection between the microstructure and radiation-induced changes during densification and swelling stages. We found that graphite swells even while lattice parameters (both a- and c-axes) shrink. We discuss the reasons for such behavior.
3:00 PM
Micro X-ray Computed Tomography of TRISO Fuel: William Chuirazzi1; Joshua Kane1; John Stempien1; Rahul Kancharla1; Fei Xu1; Nikolaus Cordes2; 1Idaho National Laboratory; 2Los Alamos National Laboratory
Before advanced nuclear reactor concepts come online to provide carbon-free energy sources, nuclear materials and fuel forms must be studied extensively for commercial qualification. While destructive examinations have been historically performed, recent developments in micro X-ray Computed Tomography (XCT), have enabled nondestructive three-dimensional (3D) examination of irradiated Tristructural isotropic (TRISO) coated fuel particles and TRISO compacts. In this work, imaging of fresh and irradiated individual TRISO particles, as well as imaging of irradiated TRISO compacts, is discussed with emphasis on the sample preparation, radiation shielding, and methodology necessary for the imaging of highly radioactive TRISO samples. The implementation of custom 3D image reconstruction techniques that allow for additional information from both the uranium-based kernel and the carbon-based buffer layers is also presented. Lastly, a discussion on quantitative data extraction and its future use in TRISO fuel analysis is included in this work.
3:20 PM Break
3:35 PM
Precipitation Microstructure of Al-Mg and Related Alloys Examined by Two-dimensional Anomalous SAXS at the K Absorption Edges of Mg and Al: Hiroshi Okuda1; Keita Aoyama2; Shan Lin2; Kazuhiko Mase3; Yusuke Tamenori4; 1Kyoto University; 2Kyoto University graduate student; 3High Energy Accelerator Organization; 4Japan Sychrotron Radiation Research Institute
Quantitative measurements of two-dimensional SAXS intensity at the K absorption edges of Mg and Al have been made for annealed Al-Mg based alloy systems. The SAXS intensity have been normalized by using secondary standard glassy carbon samples calibrated by a primary glassy carbon sample provided by Ilavsky, ANL.The contrast change at the Mg absorption edge agreed with the one expected from the anomalous dispersion of Mg. Thin glassy carbon was found to give well-defined strong scattering at the photon energy of interest. Phase boundary calculated from the normalized SAXS intensity of Al-Mg alloy agreed with the reported ones obtained by other approaches such as calorimetric measurements and thermodynamical assessments. Preliminary results applied to AlMgSi systems will be also shown.
3:55 PM
Abnormal Grain Growth and Nano-oxide Precipitation of Oxide Dispersion Strengthened Steels Throughout Their Consolidation Evaluated by In-situ Wide and Small Angle X-ray Scattering: Gabriel Spartacus1; Joël Malaplate2; Frédéric de Geuser3; Denis Sornin2; Raphaëlle Guillou2; Alexis Deschamps3; 1KTH; 2CEA Saclay; 3Univ. Grenoble Alpes
Oxide Dispersion Strengthened (ODS) steels are candidate materials for nuclear fusion and fission power plants. The production process of ODS steels includes ball milling of Fe-Cr, Y2O3 and TiH2 to dissolve Y, Ti and O into the matrix. This process also induces a very fine and deformed grain microstructure. During subsequent annealing at 1100°C, Y-Ti-O nano-oxides form, grain grows and dislocation density evolves, all in intricate ways that are so far poorly understood, mostly due to lack of experimental data. To investigate these features, both the nano-oxides precipitation and mean crystallite size and dislocation density were investigated by in-situ small and wide angle X-ray scattering respectively, monitoring the pinning of grains and dislocations by the growing nano-oxides, already effective at 500°C. The temperature of abnormal grain growth were determined on several ODS grades between 600-800°C, and different trends were identified on several ODS with different Y/Ti/O ratios addition.
4:15 PM
Investigating the Polymer Network Structure of Epoxy Thermosets Using X-ray Scattering: Derek Dwyer1; Zach Brubaker1; Sara Isbill1; Jenn Neu1; Wim Bras1; Jong Keum1; Jennifer Niedziela1; 1Oak Ridge National Laboratory
Epoxy thermosets are important structural components for high-performance carbon fiber composites. Structural changes of the epoxy polymer network from incorporated defects or imparted by thermal or mechanical stressors can cause unexpected changes in the composite performance. In this work, X-ray scattering techniques are used to investigate the polymer network structure of epoxy thermosets and investigate the resulting changes in this structure from incorporation of defects and exposure to different stressors.
4:35 PM
In-situ Neutron Diffraction Creep Behavior of Designer Superalloys Tailored for Additive Manufacturing: Patxi Fernandez-Zelaia1; Christopher Ledford1; Kira Pusch2; Evan Raeker2; Ning Zhou3; Stephane Forsik3; Austin Dicus3; Tresa Pollock2; Michael Kirka1; 1Oak Ridge National Laboratory; 2University of California, Santa Barbara; 3Carpenter Technology
Legacy alloys developed for the casting of hot section gas turbine components are notoriously difficult to weld and are not amendable to additive manufacturing (AM). AM, however, offers opportunities to open the component design space, improve engine efficiency and reduce overall emissions but it is imperative to address materials processing challenges to facilitate its adoption. In this talk, we present work on a new generation of defect-resistant high-γ’ superalloys; CoNi-based GammaPrintTM-700 and Ni-based GammaPrintTM-1100. Laser powder bed fusion samples of each alloy were subject to creep loading and in-situ neutron diffraction was utilized to measure lattice-scale deformation. The influence of precipitate-scale deformation mechanisms as well as grain-scale orientation sensitivity are discussed.