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DOE OSTI2022

V31 Test Report

The V31 containment vessel was procured by the US Army Recovered Chemical Material Directorate (RCMD) as a third - generation EDS containment vessel. It is the fifth EDS vessel to be fabricated under Code Case 2564 of the 2019 ASME Boiler and Pressure Vessel Code, which provides rules for the design of impulsively loaded vessels. The explosive rating for the vessel, based on the code case, is twenty-four (24) pounds TNT - equivalent for up to 1092 detonations. This report documents the results of explosive tests that were performed on the vessel at Sandia National Laboratories in Albuquerque, New Mexico to qualify the vessel for field operations use. There were three design basis configurations for qualification testing. Qualification test (1) consisted of a simulated M55 rocket motor and warhead assembly of 24lbs of Composition C-4 (30 lb TNT equivalent). This test was considered the maximum load case, based on modeling and simulation methods performed by Sandia prior to the vessel design phase. Qualification test (2) consisted of a regular, right circular cylinder, unitary charge, located central to the vessel interior of 19.2 lb of Composition C-4 (24 lb TNT equivalent). Qualification test (3) consisted of a 12-pack of regular, right circular cylinders of 2 lb each, distributed evenly inside the vessel (totaling 19.2 lb of C-4, or 24 lb TNT equivalent). All vessel acceptance criteria were met.

42 ENGINEERING↗

DOE OSTI2023

Microstructure and in-service degradation of baffle former bolts – in-core components of light water reactors

This report presents a microstructure evaluation of the baffle former bolt, a commercial pressurized water reactor component. Using SEM, EDS, and EBSD analysis the material was identified as AISI 316 steel with an annealed austenite microstructure. Findings include abnormal grain growth in a fraction of the grains and the absence of retained ferrite. Notable observations include an overlapping of pre- and post-irradiation deformation, including defect-free channel formation as an active deformation mechanism in the near-surface layer of BFB. Specimen surfaces, exposed to high-temperature, high-pressure water, exhibited signs of in-service corrosion degradation. EBSD and EDS analyses highlighted intergranular corrosion, possible grain boundary oxidation with depths less than 3 µm, and, unexpectedly, short cracks filled with Cr-rich oxides measuring around 5-6 µm. The presence of defect-free channels from EBSD data suggests episodes of high mechanical stresses during service. The specimens provide a potentially unique insight into the in-service degradation of NPP components, strain localization, and crack initiation processes. An intact corrosion layer reveals a complex component's in-service history. Further research is underway for a detailed analysis.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Improving qubit coherence time through detailed materials analysis

This study investigates the defects, imperfections, and variations in superconducting Nb thin films deposited on sapphire substrates. Two samples, W114 and W118, were fabricated using DC Magnetron Sputtering and Electron Cyclotron Resonance (ECR), respectively. Each sample was analyzed at five distinct spots to compare elemental homogeneity and thickness variations. Scanning Electron Microscopy (SEM) was employed to examine surface morphology, while Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) provided elemental and chemical state analyses. SEM revealed distinct structures in W114 and a uniform surface in W118. EDS showed higher aluminum and oxygen signals in W118, indicating a thicker film. XPS detected a higher Nb₂O₅ signal in W118, attributed to a thicker oxygen layer. These findings highlight the critical role of precise material characterization in advancing quantum computing technologies.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

V31 Test Report

The V31 containment vessel was procured by the US Army Recovered Chemical Materiel Directorate (RCMD) as a third-generation EDS containment vessel. It is the fifth EDS vessel to be fabricated under Code Case 2564 of the 2019 ASME Boiler and Pressure Vessel Code, which provides rules for the design of impulsively loaded vessels. The explosive rating for the vessel, based on the code case, is twenty-four (24) pounds TNT-equivalent for up to 1092 detonations. This report documents the results of explosive tests that were performed on the vessel at Sandia National Laboratories in Albuquerque, New Mexico to qualify the vessel for field operations use. There were three design basis configurations for qualification testing. Qualification test (1) consisted of a simulated M55 rocket motor and warhead assembly of 24lbs of Composition C-4 (30 lb TNT equivalent). This test was considered the maximum load case, based on modeling and simulation methods performed by Sandia prior to the vessel design phase. Qualification test (2) consisted of a regular, right circular cylinder, unitary charge, located central to the vessel interior of 19.2 lb of Composition C-4 (24 lb TNT equivalent). Qualification test (3) consisted of a 12-pack of regular, right circular cylinders of 2 lb each, distributed evenly inside the vessel (totaling 19.2 lb of C-4, or 24 lb TNT equivalent). All vessel acceptance criteria were met .

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Iodine Capture Studies of Copper- and Bismuth-Based Sorbents

The release of radioiodine, one of several radionuclides of concern when recycling used nuclear fuel (UNF), is an important consideration in the fuel cycle. In this study, two sorbent materials, Cu 0 -polyacrylonitrile (PAN) and Bi 0 -PAN, were tested as solid sorbent candidates for iodine capture. Experiments using a thin bed of sorbent material were exposed to vaporized iodine for over 300 hours (~2 weeks) under varied conditions in a dynamic flow environment. The overall performance was monitored in real-time using thermogravimetric analysis, and the materials were subsequently characterized for surface and bulk analysis using scanning electron microscopy – energy-dispersive spectroscopy (SEM-EDS) and powder x-ray diffraction (pXRD), respectively. Iodine (in the form of I 2 ) is expected to be released primarily in the dissolver off-gas (DOG) stream; therefore, this study demonstrates the effects of elemental iodine (I 2 ), water vapor (H 2 O), and nitrogen dioxide (NO 2 ). When exposed to ‘ideal’ conditions (in which I 2 is carried by dry air), Cu 0 -PAN and Bi 0 -PAN behave differently, with TGA analysis indicating that Cu 0 sorption performance is higher than that of Bi 0 , as evidenced by a larger mass change. Under ‘harsh’ conditions—such as a gaseous feed containing I 2 , H 2 O, and NO 2 vapors carried by air,—iodine capture performance for both Cu 0 - and Bi 0 -PAN are affected. SEM-EDS and pXRD analysis of these materials is discussed herein.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Multimodal Few-Shot Segmentation of Electron Micrographs

Scanning transmission electron microscopy (STEM) is one of the most used methods of analyzing the chemistry and composition of materials. By analyzing microstructures, these microscopes can help scientists better understand the molecular underpinnings of microelectronics, batteries, and more. However, STEM data can be difficult to interpret, so recent developments have been made in applications of machine learning to analyze these images. The PNNL-developed pyCHIP Classifier has achieved results in segmenting STEM these images via few-shot learning, a method which requires little data and human input, perfect for quickly analysis. In my internship I (Eli Meyers) investigated a multimodal improvement of this classifier by incorporating energy dispersive x-ray spectroscopy (EDS) data into the classification process for a more accurate segmentation. Furthermore, I encoded the spectral data by training a mass spectrometry encoder on the EDS data to extract a more meaningful representation of the data.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Gold Nanoparticles AuNP Decorated on Fused Graphene-like Materials for Application in a Hydrogen Generation

The search for a sustainable, alternative fuel source to replace fossil fuels has led to an increased interest in hydrogen fuel. This combustible gas is not only clean-burning but can readily be produced via the hydrolysis of sodium borohydride. The main drawback of this reaction is that the reaction occurs relatively slowly and requires a catalyst to improve efficiency. This study explored a novel composite material made by combining gold nanoparticles and fused graphene-like materials (AuFGLM) as a catalyst for generating hydrogen via sodium borohydride. The novel fused graphene-like material (FGLM) was made with a sustainable dextrose solution and by using a pressure-processing method. Imaging techniques showed that FGLM appears to be an effective support template for nanoparticles. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and Raman spectroscopy were used to characterize and determine the size, shape, and structure of nanoparticles and composites. The TEM study characterized the fused carbon backbone as it began to take on a rounder shape. The TEM images also revealed that the average diameter of the gold nanoparticle was roughly 23 nm. The FTIR study confirmed O-H, C-C, and C=O as functional groups in the materials. The EDS analysis showed that the composite contained approximately 6.3% gold by weight. The crystal structures of FGLM and AuFGLM were identified via P-XRD analysis. Various reaction conditions were used to test the catalytic ability of AuFGLM, including various solution pHs, temperatures, and doses of NaBH 4 . It was observed that optimal reaction conditions included high temperature, an acidic solution pH, and a higher dose of NaBH 4 . The activation energy of the reaction was determined to be 45.5 kJ mol -1 , and it was found that the catalyst could be used multiple times in a row with an increased volume of hydrogen produced in ensuing trials. The activation energy of this novel catalyst is competitive compared to similar catalysts and its ability to produce hydrogen over multiple uses makes the material an exciting choice for catalyzing the hydrolysis of NaBH 4 for use as a hydrogen fuel source.

08 HYDROGEN↗

DOE OSTI2022

High-Resolution Transmission Electron Microscopy Study of a Powder River Basin Coal-Derived Fly Ash

Examination of a fly ash derived from the combustion of a low-S, subbituminous Powder River Basin coal by Scanning Electron Microscopy (SEM) and High-resolution Transmission Electron Microscopy (HRTEM), both supplemented by Energy-dispersive X-ray spectroscopy (EDS), showed that the fly ashes were dominated by amorphous phases, Ca-rich plagioclase feldspars, Mg-rich phases, complex Ca-Mg-Al-Si-Ti-Fe grains, and trace amounts of REE-rich particles. Many of the particles were rimmed by a Ca-S, possibly a sulfate. HRTEM-EDS examination of a REE-rich particle proved it to be a mix of light- and heavy-rare earth minerals mixed with amorphous phases.

58 GEOSCIENCES↗

DOE OSTI2025

Probing the Critical Element Chemistry of Coal-Combustion Fly Ash: Examination of Zircon and Associated Minerals from a Beneficiated Kentucky Fly Ash

Along with the principal rare earth (REE) minerals such as monazite, xenotime, and bastnasite, Y-and REE-bearing zircon and associated minerals survive the combustion process and are found in coal-combustion fly ash. Beneficiated fly ash from a power plant burning an eastern-Kentucky-sourced coal blend was found to have zircon (ZrSiO4), baddeleyite (ZrO2), fergusonite (YNbO4), yttriaite (Y2O3), and xenotime (YPO4). Previous studies of the same fly had also identified monazite with a broad REE suite. Scanning electron microscopy–electron dispersive spectroscopy (EDS) and transmission electron microscopy (TEM)–EDS as well as other TEM-based techniques revealed a variety of zircon associations, including heavy-REE suites with Y, Nb, and Hf. Hafnium is a common accessory element in zircons and the Y and Nb may be present as fergusonite (YNbO4) intermixed with zircon.

Berti, Debora (ORCID:0000000311237794)↗

DOE OSTI2022

Combinatorial Cu-Ni Alloy Thin-Film Catalysts for Layer Number Control in Chemical Vapor-Deposited Graphene

We synthesized a combinatorial library of CuxNi1−x alloy thin films via co-sputtering from Cu and Ni targets to catalyze graphene chemical vapor deposition. The alloy morphology, composition, and microstructure were characterized via scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), and X-ray diffraction (XRD), respectively. Subsequently, the CuxNi1−x alloy thin films were used to grow graphene in a CH4-Ar-H2 ambient at atmospheric pressure. The underlying rationale is to adjust the CuxNi1−x composition to control the graphene. Energy dispersive x-ray spectroscopy (EDS) analysis revealed that a continuous gradient of CuxNi1−x (25 at. % < x < 83 at.%) was initially achieved across the 100 mm diameter substrate (~0.9%/mm composition gradient). The XRD spectra confirmed a solid solution was realized and the face-centered cubic lattice parameter varied from ~3.52 to 3.58 A˙, consistent with the measured composition gradient, assuming Vegard’s law. Optical microscopy and Raman analysis of the graphene layers suggest single layer growth occurs with x > 69 at.%, bilayer growth dominates from 48 at.% < x < 69 at.%, and multilayer (≥3) growth occurs for x < 48 at.%, where x is the Cu concentration. Finally, a large area of bi-layer graphene was grown via a CuxNi1−x catalyst with optimized catalyst composition and growth temperature.

2D materials↗

DOE OSTI2024

Focused Ion Beam Tomography of Alloy 617 Corroded in Molten Chloride Salt

Materials qualification of reactor structural materials is a critical step in rapid implementation of advanced nuclear reactor technologies, particularly to assess the corrosion performance in these designs. Accelerated qualification of reactor structural materials requires incorporating powerful computational toolsets, such as phase field modelling in the Multiphysics Object-Oriented Simulation Environment (MOOSE) framework, to predict the evolution of structural materials due to corrosion. Accordingly, computational toolsets will require experimental data generated at appropriate length scales to validate accuracy. Focused ion beam (FIB) provides a high degree of control over manipulation of materials for analytical purposes, including capturing data on the evolution in the microstructure and elemental composition of materials at the mesoscale, an appropriate length scale for phase field modelling of intergranular diffusion phenomena using the MOOSE framework. For instance, the FEI Helios G4 UX dual beam plasma FIB microscope at the Irradiated Materials Characterization Laboratory (IMCL) is capable of backscatter diffraction (EBSD) and energy-dispersive x-ray spectroscopy (EDS) documenting the evolution in the microstructure and elemental composition, respectively. The Helios can perform EDS and EBSD three-dimensionally (3D) using tomography, which is then combined using different software packages to visualize 3D volumes correlating elemental composition to microstructural data. The purpose of this investigation was to develop a streamlined characterization and data processing workflow for 3D tomography studies on the FEI Helios G4 plasma FIB. The investigation is segmented into three parts: 1) Optimizing the data collection workflow, 2) identifying appropriate data processing and visualization software (i.e. DREAM.3D, MIPAR, and VGStudioMax), and 3) establishing an infrastructure for public release. The optimization of the data collection workflow is in collaboration with members of the U220 department to setup formal training on the tomography operation of the G4, through ThermoFisher Scientific, and exploring DREAM.3D, MIPAR, and VGStudioMax data processing/visualization software packages. VGStudioMax currently demonstrates the most promise for future use. Optimization of the data collection and processing workflow is still ongoing. A collaboration with INL High Performance Computing (HPC) established an open-source license for expediting the public release of FIB tomography datasets through HPC. FIB tomography data generated by the G4 will provide comprehensive data for validating 3D phase field mesoscale modelling tools within the MOOSE framework for accelerated qualification of reactor structural materials.

Copeland-Johnson, Trishelle↗

DOE OSTI2024

Corrosion of Zinc Cold Spray Coatings in a Wet Sweet and Sour Gas Environment

Internal corrosion is a problem for steel pipelines transporting natural gas or CO 2 containing water and partial pressures of H 2 S higher than 0.3 kPa (0.05 psi). This work aims to mitigate internal corrosion in steel pipelines transporting natural gas containing H 2 S using cold spray coatings. Two types of the cold spray binary metallic coatings (zinc chromium [ZnCr]. zinc niobium [ZnNb]) were studied using electrochemical techniques: potentiodynamic polarization, linear polarization resistance, and electrochemical impedance spectroscopy. The corrosion resistance of cold spray coatings (ZnCr, ZnNb) was evaluated in an environment containing 4 bar CO 2 pressure, simulating the partial pressures found in gas transmission lines over a solution of 3.5 wt% NaCl heated to 40°C. A concentration of 0.003 M Na 2 S 2 O 3 ·5H 2 O, corresponding to H 2 S partial pressures around 0.079 bar (1.146 psi), was used to simulate sour conditions. Postcorrosion surface characterization was performed using a scanning electron microscope (SEM) equipped with an energy-dispersive x-ray spectroscope (EDS) and x-ray diffraction analysis. The data showed that the presence of 0.003 M Na 2 S 2 O 3 ·5H 2 O shifted the corrosion potential to more anodic values and decreased the corrosion current density. Both coatings showed similar behavior after 1 h of exposure in the CO 2 /H 2 S environment, indicating that similar electrochemical reactions were occurring on ZnNb and ZnCr. SEM images and EDS surface analyses for specimens showed a significant change in the surface chemical composition of carbon steel coated with ZnNb and ZnCr after 24 h of immersion. In the presence of thiosulfate (under sour conditions), the formation of corrosion product layers (ZnCO 3 and ZnS) on top of ZnNb and ZnCr coatings increased their corrosion resistance, which helped to reduce their corrosion by a factor of 2. Under a sweet environment, the corrosion rates for steel coated with cold spray coatings after 14 d of exposure are lower than that for galvanized steel by a factor of 5 due to the ZnCO 3 layer formed on top of the coatings. The ZnCO 3 layer formed on the steel surface acts as a physical barrier against corrosion by blocking the diffusion of corrosive species to the surface. No localized attack was observed. ZnCr Cold spray coating with defect showed promising corrosion protection against CO 2 corrosion (sweet corrosion) after 14 d of exposure to a CO 2 environment. Here, the scratch on the coating simulated damage created in service, and it was deep enough to expose the substrate material (steel). The formation of zinc oxide (ZnO) and zinc carbonate (ZnCO 3 ) on the scratch confirmed the cathodic protection of the steel by ZnCr and ZnNb coatings.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Solving the Dynamics-Aware Economic Dispatch Problem with the Koopman Operator

The dynamics-aware economic dispatch (DED) problem embeds low-level generator dynamics and operational constraints to enable near real-time scheduling of generation units in a power network. DED produces a more dynamic supervisory control policy than traditional economic dispatch (T-ED) that reduces overall generation costs. However, in contrast to T-ED, DED is a nonlinear, non-convex optimization problem that is computationally prohibitive to solve. We introduce a machine learning-based operator-theoretic approach for solving the DED problem efficiently. Specifically, we develop a novel discrete-time Koopman Operator (KO) formulation that embeds domain information into the structure of the KO to learn high-fidelity approximations of the generator dynamics. Using the KO approximation, the DED problem can be reformulated as a computationally tractable linear program (abbreviated DED-KO). We demonstrate the high solution quality and computational-time savings of the DED-KO model over the original DED formulation on a 9-bus test system.

King, Ethan↗

DOE OSTI2021

Microstructural and Micro-Chemical Evolutions in the Irradiated UCO Fuel Kernels of AGR-1 and AGR-2 TRISO Fuel Particles

AGR-1 and AGR-2 TRISO fuel particles were fabricated with slightly different fuel kernel chemical compositions, modified fabrication processes, different fuel kernel diameters, and changed 235U enrichments. To correlate those differences with the fuel kernel responses to neutron irradiations in terms of irradiated fuel microstructure, fission products chemical and physical states, and fission gas bubble evolutions, extensive microstructural and analytical characterizations were conducted. The studies used a state of art transmission electron microscopy (TEM) equipped with Energy-dispersive X-ray spectroscopy (EDS) of four silicon solid-state detectors which have super sensitivity and fast speed. The TEM specimens were prepared from selected AGR-1 and AGR-2 irradiated fuel kernels exposed to safety testing after irradiation. The particles were chosen to represent a representative irradiation conditions with a fuel burnup within the range from 10.8 to 18.6% FIMA, and the time-average volume-average temperatures vary from 1070 to 1287°C. The 235U enrichment was 19.74 wt.% for the AGR1 fuel kernels and 14.03 wt.% for the AGR-2 fuel kernels. The TEM results show that there were significant microstructural reconstructions in the irradiated fuel kernels for both the AGR-1 and AGR-2 fuels. There are four major phases including fuel matrix of UO2 and UC, U2RuC2, and UMoC2 in the irradiated AGR2 fuel kernel. Zr and Nb form solid solution in the UC phase. UMoC2 phase often shows a detectable concentration of Tc. Pd was found to mainly locate in the buffer layer or to be associated with fission gas bubble within the UMoC2 phase. The EDS maps qualitatively show that the rare-earth fission products (Nb, et al.) preferentially reside in the UO2 phase. In contrast, in the irradiated AGR1 fuel kernel, no U2RuC2 or UMoC2 precipitates were positively identified. Instead, there is a high number of rod-shape precipitates enriched with Ru, Tc, Rh, and Pd observed in the fuel kernel center and edge zone. The difference of microstructural and micro-chemical evolutions in irradiated fuel kernels between the AGR-1 and AGR-2 TRISO fuel particle may result from a combined factor of irradiation temperature, fuel geometry and chemical composition. However, the irradiation temperature probably play a more deterministic role. Limited electron energy loss spectroscopy (EELS) characterizations on the AGR2 fuel kernel show that there is nearly no carbon in the UO2 phase while a small fraction of oxygen was detected in the UC/UMoC2 phase.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Improving Qubit Coherence Time Through Detailed Materials Analysis

This study investigates the defects, imperfections, and variations in Nb thin films deposited on sapphire substrates. Two samples, W114 and W118, were fabricated using DC Magnetron Sputtering and Electron Cyclotron Resonance (ECR), respectively. Each sample was analyzed at five distinct spots to compare elemental homogeneity and variations in oxide layers. Scanning Electron Microscopy (SEM) was employed to examine surface morphology, while Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Photoelectron Spectroscopy (XPS) provided elemental and chemical state analyses. SEM revealed distinct structures in W114 and a uniform surface in W118. EDS showed higher aluminum signals in W118, indicating a thinner film in comparison to W114. XPS detected a higher Nb₂O₅ signal in W118, in comparison to W114, which can be attributed to the presence of a thicker Nb₂O₅ layer in W118. These findings highlight the critical role of precise material characterization in advancing quantum computing technologies.

Rosado Bonilla, Cristy M.↗

DOE OSTI2025

Elucidating the corrosion mechanism of Ni-based superalloys in the presence of uranium-containing chloride molten salt

The United States Department of Energy (DOE) is committed to the advancement of nuclear reactor technology through initiatives such as the Advanced Reactor Development Program (ARDP), in an effort to diversify the United States energy portfolio towards more sustainable energy options. The ARDP includes demonstration by industry partners of molten chloride fast reactors (MCFRs). Construction of MCFRs requires qualified nuclear structural materials. Unfortunately, there are no current materials that are fully qualified by the Nuclear Regulatory Commission for the construction of molten salt reactors, including MCFRs. Adapting current structural material qualifications requires expansion of our current knowledgebase on the property-performance relationships regarding corrosion performance. In this investigation, we assess microstructural changes in a Ni-based superalloy after exposure to a UCl3¬-containing chloride salt eutectic mixture through a correlated multi-modal approach combining several advanced characterization techniques, including scanning electron microscopy/focused ion beam (SEM/FIB) and transmission electron microscopy (TEM). SEM/FIB analysis will illustrate changes in elemental composition, microstructure, and isotopic information acquired from energy x-ray dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and secondary ion mass spectroscopy (SIMS), respectively. This information will then aid in identifying localized regions to elucidate the corrosion mechanism with TEM through a combination of electron diffraction, electron energy loss spectroscopy (EELS), and additional EDS. The findings from this investigation will further expand our assessment of the corrosion performance of structural materials in molten salt chloride systems, aiding to developing fully qualified materials for construction of MCFRs.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Understanding Fission Gas Bubble Distribution and Zirconium Redistribution in Neutron-irradiated U-Zr Metallic Fuel Using Machine Learning

U-10wt.% Zr (U-10Zr) based metallic fuel is the leading candidate for next-generation sodium cooled fast reactor in United States. Currently, Idaho National Laboratory (INL) has been the leading national laboratory for research, development, and demonstration (RD&D) on metallic fuel. Advanced post-irradiation characterization will help to understand fuel microstructure and property change during irradiation, benefiting fuel qualification for commercial application. Characterization capabilities ranging from sub-nanometer to micrometer, such as scanning electron microscopy (SEM), focused ion beam (FIB) sampling, transmission electron microscopy (TEM) characterization, and local thermal conductivity microscopy (TCM), have been utilized recently on irradiated U-10Zr fuel samples to gain a better understanding of nuclear fuel microstructure and property evolution inside a reactor. The FIB/SEM coupled with energy dispersive X-ray spectroscopy (EDS) can capture the essential information to achieve better understanding of fuel behaviors. Inside a nuclear reactor, the phase and microstructure of U-10Zr is constantly changing under neutron bombardment. For example, the gaseous fission product atoms have a limited solubility inside fuel matrix and tend to precipitate out in bubble form, which not only contribute to fuel thermal conductivity degradation but also provide a shortcut for movement of fission products, i.e. lanthanides. The resultant deposition of lanthanides at the cladding inner surface will potentially trigger a chemical reaction/interaction between nuclear fuel and cladding at reactor operational conditions, threatening fuel integrity and safety. FIB/SEM coupled with EDS can provide the fission bubble information as well as probe into phase separation or Zr redistribution, which is fundamental to predict the fuel performance. With high velocity image data generating method, such as FIB/SEM, an automatic way to extract the microstructural information quantitively can better serve the needs from post irradiation characterization. A trained machine learning model, named Decision Tree, is employed to generate a bubble classifier and to categorize bubbles into three categories: isolated bubble, connected without lanthanides, and connected with lanthanides bubbles[3]. This work presents a showcase of this approach on six regions of a fuel cross-section along the radial temperature gradient. We obtained distributions of bubble categories and porosity rates along the six regions. Moreover, a secondary phase U-Zr2 was determined and found on regions 5 and 6. The secondary phase fraction was increasing from 15.61% in region 5 to 34.79% in region 6 based on this approach . This quantitative data offers insights into the lanthanide migration and potentially thermal conductivity degradation. This information from machine learning will be fed into fuel design code for better prediction of fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

DED Additively Manufactured HEAs Optimized via Parametric Study of Functionally Graded Materials

Complex concentrated alloys (CCAs) are a system of alloys composition of nearly equiatomic elements, creating a state of high configurational entropy in the material. These alloys are of interest for various industrial applications due to their high strength and hardness, wide operational temperature range, creep and diffusion resistance, and radiation resistance. In the current work CoCrFeNi-base CCAs are synthesize by combining three commonly industrial alloys: IN718, SS316L, and 70Co30Cr (commercially known as Stellite 21), in-situ utilizing directed energy deposition (DED) additive manufacturing (AM). One bulk specimen is fabricated with a 1:1:1 ratio of IN718, SS316L, and 70Co30Cr where IN718 is a source of nickel and chrome, SS316 is a source of iron and chrome, and 70Co30Cr is a source of cobalt and supplemental chrome. Additionally, a functionally graded material (FGM) of the identified CCA system from SS316 was fabricated with 10 layers, where the initial five layers are the base material of SS316L and graded by steps of 20% to transition to the CCA system. Overall build quality, microstructure, compositional distribution, phases analysis, and microhardness were studied by laser optical microscopy, scanning election microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction analysis (XRD), and Vickers microhardness techniques. Overall build quality showed a successful bulk build with acceptable density, however unmelted particles are observed in the as-built alloy. Compositional results show that the system meets the Boltzmann’s hypothesis definition of an HEA, and that an FCC CCA was produced with increased hardness, small grain size, and superior hardness properties to the SS316L substrate. While initial XRD results show predominately FCC structure, EDS analysis of interdendritic regions show the existence of Laves phases in the material. The fabrication of an FGM CCA allowed for potential screening of additional alloy mixes which may be of interest to explore in future research, and the resulting composition is compared to predicted values. This novel method of CCA fabrication results in substantial cost savings of these CCA systems over traditional methods.

36 MATERIALS SCIENCE↗