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At least 289 records · Page 16

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DOE OSTI2020

An Overview of Neutron Irradiated SiC Layer Behavior using Micro-and Nano-Characterization Techniques

The complexity of fission product distribution and composition within the SiC layer of tristructural isotropic (TRISO) coated particles, irradiation effects on the SiC structure as well as the variable nature of metallic fission product release, has led to the exploration of multiple micro- and nano-characterization techniques. The fine scale of the fission product precipitates necessitates unique learnings and application of electron microscopic techniques with irradiated fuel during the Advanced Gas Reactor (AGR)-1 experiment analysis. A summarized discussion on the specific advanced techniques with associated method development for TRISO coated particles is provided followed by the down selected techniques currently considered to provide the highest impact. Techniques considered are electron probe micro-analyzer (EPMA), scanning transmission electron microscopy (STEM), and Precession electron diffraction (PED). SiC grain boundary characteristics are evaluated due to the mobility of specific fission products through grain boundaries. PED was performed for understanding the role of grain boundary character on fission product transport. One set of comparative analyses between AGR-1 and AGR-2 particles leads to a finding that the AGR-1, high-Ag-retention particle, had statistically more coincidence site lattice (CSL)-related grain boundaries (but fewer low-angle grain boundaries), compared to the AGR-2 particle. This implies that CSL-related grain boundaries may have a direct influence on Ag retention. However, precipitates were found on a relatively small fraction of CSL-related grain boundaries in both particles. In another set of comparison between AGR-1 and AGR-2 particles that were subjected to safety testing, there is significant differences in average SiC grain boundary distributions, but the fission product distributions on these grain boundaries are very similar.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Micro- and Nano-techniques for the Study of Fission Product Precipitation in SiC Layer

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Enhanced Interfacial Electron Transfer in Photocatalyst-Natural Enzyme Coupled Artificial Photosynthesis System: Tuning Strategies and Molecular Simulations

Laccase is capable of catalyzing a vast array of reactions, but its low redox potential limits its potential applications. The use of photocatalytic materials offers a solution to this problem by converting absorbed visible light into electrons to facilitate enzyme catalysis. Herein, MIL-53(Fe) and NH 2 -MIL-53(Fe) serve as both light absorbers and enzyme immobilization carriers, and laccase is employed for solar-driven chemical conversion. Electron spin resonance spectroscopy results confirm that visible light irradiation causes rapid transfer of photogenerated electrons from MOF excitation to T1 Cu(II) of laccase, significantly increasing the degradation rate constant of tetracycline (TC) from 0.0062 to 0.0127 min -1 . Conversely, there is only minimal or no electron transfer between MOF and laccase in the physical mixture state. Theoretical calculations demonstrate that the immobilization of laccase's active site and its covalent binding to the metal-organic framework surface augment the coupled system's activity, reducing the active site accessible from 27.8 to 18.1 Å. In conclusion, the constructed photo-enzyme coupled system successfully combines enzyme catalysis’ selectivity with photocatalysis's high reactivity, providing a promising solution for solar energy use.

36 MATERIALS SCIENCE↗

DOE OSTI2025

In-situ ion irradiation of fission products in a spent UO 2 fuel

This study investigates the behavior of fission gas bubbles and five metal precipitates (5MPs) (Mo, Ru, Rh, Tc, Pd) in spent uranium dioxide (UO 2 ) fuel under various ion irradiation doses, temperatures, and flux conditions. Utilizing in-situ ion irradiation and advanced transmission electron microscopy, we analyzed the evolution of fission gas bubbles and 5MPs in UO 2 samples from the Belgium Reactor 3 (BR-3). Our findings reveal significant shrinkage of fission gas bubbles and 5MPs with increasing irradiation dose, accompanied by a decrease in pair density. We demonstrate that ion irradiation induces a homogeneous re-solution process where individual atoms are ejected from bubbles and precipitates, leading to their dissolution and subsequent re-precipitation in the matrix. In conclusion, this study provides critical insights into the dynamic behavior of fission products under irradiation, facilitating the development of predictive models and contributing to the optimization of nuclear fuel performance and safety.

Fission products↗

DOE OSTI2023

Ion emission from warm dense matter produced by irradiation with a soft x-ray free-electron laser

Here we report on an experiment performed at the FLASH2 free-electron laser (FEL) aimed at producing warm dense matter via soft x-ray isochoric heating. In the experiment, we focus on study of the ions emitted during the soft x-ray ablation process using time-of-flight electron multipliers and a shifted Maxwell–Boltzmann velocity distribution model. We find that most emitted ions are thermal, but that some impurities chemisorbed on the target surface, such as protons, are accelerated by the electrostatic field created in the plasma by escaped electrons. The morphology of the complex crater structure indicates the presence of several ion groups with varying temperatures. We find that the ion sound velocity is controlled by the ion temperature and show how the ion yield depends on the FEL radiation attenuation length in different materials.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

Irradiation Creep and Fatigue Observed via In-situ Electron Microscopy.

Abstract not provided.

Hattar, Khalid↗

DOE OSTI2025

In-situ ion irradiation of a spent UO2 fuel: evolution of fission products and nanograins with radiation dose

This study investigates the behavior of fission gas bubbles, five metal precipitates (5MPs) (Mo, Ru, Rh, Tc, Pd) and nanograins in spent uranium dioxide (UO2) fuel under various ion irradiation doses, temperatures, and flux conditions. Utilizing in-situ ion irradiation and advanced transmission electron microscopy, we analyzed the evolution of fission gas bubbles, 5MPs and nanograins in UO2 samples from the Belgium Reactor 3 (BR-3). Our findings reveal significant shrinkage of fission gas bubbles and 5MPs with increasing irradiation dose, accompanied by a decrease in pair density. The study also reveals nanograin coarsening under irradiation. We demonstrate that ion irradiation induces a homogeneous re-solution process where individual atoms are ejected from bubbles and precipitates, leading to their dissolution and subsequent re-precipitation in the matrix. This study provides critical insights into the dynamic behavior of fission products and nanograins under irradiation, facilitating the development of predictive models and contributing to the optimization of nuclear fuel performance and safety.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Void shrinkage in 21Cr32Ni austenitic model alloy during in-situ ion irradiation

Austenitic 21Cr32Ni model alloy thin foils, previously irradiated with 5 MeV Fe ++ ions in bulk to create voids, were re-irradiated in-situ in the Intermediate Voltage Electron Microscope Facility (IVEM). The voids which had been formed under bulk-ion irradiation shrank and disappeared after in-situ Kr ion irradiation in the temperature range 50 K-713 K to an additional dose of 1 dpa. The voids were unaffected by eithersuccessive thermal annealing to 673 K and by prolonged exposure to the 200 keV electron beam at the irradiation temperature. The high void shrinkage rate observed did not change significantly for irradiation temperatures between 50 K and 713 K, suggesting that the void shrinkage process in thin foils during in-situ heavy-ion irradiation results from the interactions of displacement cascades with the voids. Finally, possible void shrinkage mechanisms under thin foil irradiation are discussed in this study.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Patch-Based Convolutional Neural Networks for Multiple Microstructural Features Detection in FIB-SEM Micrographs of Irradiated Nuclear Fuel

Focused ion beam scanning electron microscopy (FIB-SEM) tomography has increasingly been utilized for acquiring three-dimensional (3D) microstructure features at the sub-micron scale in irradiated nuclear materials. This technique involves sequential ion beam slicing followed by electron beam imaging and compositional mapping using energy dispersive spectroscopy (EDS). Despite its growing use, several challenges persist. These include the time-intensive nature of data collection of EDS data, difficulties in distinguishing between various microstructures, and issues with image alignment. These challenges currently limit the broader application of FIB-SEM tomography in the field. To overcome these limitations, we propose using convolutional neural networks (CNNs) to automate microstructure identification in SEM images. Our study introduces a new framework for identifying microstructures in irradiated U-10Zr (wt. %) metallic fuel with limited annotated data. The framework includes the creation of a reliable annotated dataset with paired SEM and ground truth data from EDS maps, the applications of CNNs for microstructure identification, and the validation of model performance. Specifically, we employed the Segment Anything Model (SAM) to align SEM images with corresponding EDS maps and focused ion beam (FIB) tomography SEM data. We evaluate several models, including Patch-based U-Net, Attention U-Net, and Residual U-Net, finding that patch-based U-Net exhibits superior segmentation performance and consistency. This approach reduces reliance on EDS detectors and aids in accelerating nuclear material analysis process, highlighting the potential of advanced deep learning techniques to improve microstructural understanding in nuclear material. This is the first framework to integrate SAM and Patch-based CNN models for semantic segmentation of irradiated nuclear materials, with potential applicability to other tomography datasets.

36 - MATERIALS SCIENCE↗

DOE OSTI2022

Role of electronic energy loss on defect production and interface stability: Comparison between ceramic materials and high-entropy alloys

High-entropy alloys (HEAs) and some complex alloys exhibit desirable properties and significant structural stability in harsh environments, including possible applications in advanced reactors. Energetic ion irradiation is often used as a surrogate for neutron irradiation; however, the impact of ion electronic energy deposition and dissipation is often neglected. Moreover, differences in recoil energy spectrum and density of cascade events on damage evolution must also be considered. In many chemically complex alloys, the mean free path of electrons is reduced significantly, thus their decreased thermal conductivity and slow dissipation of localized radiation energy can have noticeable effects on displacement cascade evolution that is greatly different from metals with high thermal conductivity. In this work, nanocrystalline HEAs of Ni 20 Fe 20 Co 20 Cr 20 Cu 20 and nonequiatomic (NiFeCoCr) 97 Cu 3 , both having much lower room-temperature thermal conductivity than pure Ni or Fe, are chosen as model HEAs to reveal the role that electronic energy loss during ion irradiation has in complex alloys. The response of nanocrystalline HEAs is investigated under irradiation at room temperature using MeV Ni and Au ions that have different ratios of electronic energy to damage energy, which is the energy dissipated in displacing atoms. Different from previously reported amorphization of nanocrystalline SiC, experimental results on these HEAs show that, similar to the process in nanocrystalline oxide materials, both inelastic thermal spikes via electron–phonon coupling and elastic thermal spikes via collisions among atomic nuclei contribute to the overall grain growth. The growth follows a power law dependence with the total deposited ion energy, and the derived value of the power-exponent suggests that the irradiation-induced instability at and near grain boundaries leads to local rapid atomic rearrangements and consequently grain growth. The high power-exponent value can be attributed to the sluggish diffusion and delayed defect evolution arising from the chemical complexity intrinsic to HEAs. Here, this work calls attention to quantified fundamental understanding of radiation damage processes beyond that of simplified displacement events, especially in simulating neutron environments.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Irradiation stability and thermomechanical properties of 3D-printed SiC

Neutron irradiation tests were carried out on 3D-printed SiC derived from binderjet additive manufacturing and chemical vapor infiltration. Irradiation was carried to 2.3 dpa over a temperature range of 400–850 °C. Anisotropy that had been observed in the thermal conductivity of 3D-printed SiC prior to irradiation vanished after irradiation as the irradiation defect thermal resistivity accumulated in the material. No degradation in strength was observed in the material before or after irradiation, at various temperatures, or in different orientations. Electron microscopy of the microstructure after neutron irradiation showed distinct defect morphologies in the heterogenous material, but no evidence for irradiation-induced cracking or degradation in the microstructure was observed.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Detection of coherent optical phonons in a thin bismuth film by ultrafast electron diffraction

Coherent dynamics of lattice oscillations in a ∼20-nm-thick film obtained by thermal sputtering of bismuth is studied using ultrashort electron bunches synchronised with femtosecond laser pulses irradiating the sample. The Fourier analysis of ultrafast electron diffraction (UED) data shows that the observed modulation of the signal is due to the ensemble of modes corresponding to optical phonons with frequencies of approximately 3, 6 and 9 THz. A conclusion is made that these peaks correspond to the manifestation of the bismuth A{sub 1g} mode (three-terahertz peak), as well as its first and second overtones, which is probably due to quantum confinement in a 20-nm Bi nanostructure. The possibility of a detailed study of the quantum-size effect in bismuth with the help of a transmission UED is analysed. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2021

Mechanical and Thermophysical Properties of 3D-Printed SiC before and after Neutron Irradiation – FY21

This report presents the mechanical and thermophysical properties of 3D-printed SiC before and after neutron irradiation that have been evaluated to assess the fuel matrix material for the Transformational Challenge Reactor (TCR). The TCR fuel form consists of an additively-manufactured silicon carbide (SiC) matrix and uranium nitride tristructural isotropic (UN TRISO) fuel particles, which is manufactured through a newly developed processing route combining binderjet 3D printing, TRISO fuel particle loading, and chemical vapor infiltration (CVI). Because the fuel matrix is a primary component of the TCR core and its response to mechanical and thermal loads during operation is one of the most influential factors on the integrity of TCR core, testing and evaluation have focused on producing mechanical and thermophysical properties data for the binderjet/CVI SiC. Baseline mechanical and thermophysical properties were measured from the disk specimens printed for different and sizes orientations, which included equibiaxial flexural failure strength, elastic constants, thermal diffusivity and conductivity, density, and the coefficient of thermal expansion. Flexural failure strength datasets showed similar Weibull distributions regardless of sample variants including different orientations. The mean failure strengths of the 3D-printed SiC variants were in the range of 280–310 MPa, which are slightly lower than that of the chemical vapor deposition (CVD) SiC. Thermophysical test results showed that specific heat and thermal expansion are not sensitive to the build direction of SiC samples, while thermal conductivity is highly dependent on the build direction and can be correlated to the anisotropic character of the 3D-printed SiC. Neutron irradiation tests were carried out on the 3D-printed 6-mm diameter SiC disk specimens. Irradiation was carried to 2.3 dpa over a temperature range of 360–880°C. No significant degradation in strength was observed in SiC after irradiations in various conditions and with different orientations. Anisotropy that had been observed in the thermal conductivity of 3D-printed SiC prior to irradiation vanished after irradiation as the irradiation defect thermal resistivity accumulated in the material. Electron microscopy of the microstructure after neutron irradiation showed distinct defect morphologies in the heterogenous material, but no evidence for irradiation-induced cracking or degradation in the microstructure was observed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Surprisingly high irradiation-induced defect mobility in Fe 3 O 4 as revealed through in situ transmission electron microscopy

Radiation-induced defects are expected to change the corrosion kinetics when a material is exposed to a corrosive environment. Characterization of the defects forming under irradiation and their ability to move/diffuse is therefore key to understanding how they impact the corrosion kinetics and possibly mechanisms. For that matter, Fe/Fe 3 O 4 interfaces were irradiated using 1 MeV Kr 2+ at temperatures of 273 K (25 °C), 573 K (300 °C) and 773 K (500 °C) to a maximum dose of 10 dpa (as measured in the Fe matrix) in situ in a transmission electron microscope. The evolution of the microstructure was followed as a function of the dose and temperature. The formation of defects was followed in the metal and the oxide as well as at the metal/oxide interface and characterized in terms of size and density. Additionally, the dynamic observation of the spatial distribution of the defects allowed for a qualitative assessment of the mobility of defects in the oxide as a function of temperature, revealing evidence for enhanced mobility even more so than in the Fe matrix. Mechanisms of induced defect mobility in the spinel are discussed to account for the observations.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Conjugate Heat Transfer Analysis in Pressurized Helium Gas Cooling Channels

Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 from the irradiation of Mo-100 targets. The NMR target consists of an Inconel window that allows the electron beam to penetrate and irradiate a stack of Mo-100 disks. The irradiation process generates large amounts of heat and is cooled using pressurized helium gas flowing at 400 g/s. LANL provides both numerical analysis support and experimental support. Computational fluid dynamics (CFD) and conjugate heat transfer (CHT) analysis are performed on the NMR target to analyze the helium flow and volumetric heating through the NMR system. In this iteration of numerical analysis, we update the Mo-100 disk thickness to 0.74 mm and the gap between the Inconel window and the first disk to 0.69 mm. Estimates of the heat flux from the electron beams from Monte Carlo N-Particle code (MCNP) analysis were combined with CFD to perform the CHT analysis. The pressure drop through the targets, force applied on the first disk, beam window and target disk temperatures are some of the quantities estimated using the simulations. The pressure drop through the target was estimated as 0.198 MPa, while the force due to venturi effects across the first disk was estimated to be 100 N. The results show maximum window temperatures over 600 °C and peak disk temperatures over 1600 °C. Past work has shown that beyond 650-700 °C, the Inconel window becomes susceptible to yield and rupture. The increased temperature in these results reduces the margin of error possible on beam spot size. The disk temperatures showed a sinusoidal distribution with the 6 th – 8 th disk from each window exhibiting highest disk temperatures. The peak temperature of the stainless steel housing was close to 316 °C and that of the laminations and spacers was approximately 582 °C.

43 PARTICLE ACCELERATORS↗

DOE OSTI2023

Numerical Analysis and Flow Induced Vibration Studies in Pressurized Helium Gas Cooling Channels

Los Alamos National Laboratory (LANL) is working with NorthStar Medical Radioisotopes (NMR) on their efforts to produce Mo-99 from the irradiation of Mo-100 targets. The NMR target consists of an Inconel window that allows the electron beam to penetrate and irradiate a stack of Mo-100 discs. The irradiation process generates large amounts of heat and is cooled using pressurized helium gas flowing at 400 g/s. LANL provides both numerical analysis support and experimental support. Computational fluid dynamics (CFD) simulations for both 300 g/s and 400 g/s are performed on the NMR target to analyze the helium flow through the NMR system. The pressure drop, the mass flow rate through each of the disc and window channels and the force applied on the first disc are some of the quantities estimated using CFD. These results will be combined with Monte Carlo N-Particle (MCNP) estimates of heat flux into the system from the electron beam to perform conjugate heat transfer analysis (CHT). The experiments presented in this report focus on the effect of the flow induced vibrations from helium flowing through the coolant gaps between the discs. There is concern that the flow induced vibrations may lead to excessive mass loss of the enriched Mo-100 discs, and the goal would be to mitigate the mass loss. This work presents benchtop tests of flow through a subset of the target stack which involves high speed imaging and displacement measurements used to estimate disc vibration, as well as mass loss.

42 ENGINEERING↗

DOE OSTI2022

The role of Cr concentration and temperature on cavity swelling with co-injected helium in dual-ion irradiated Fe and Fe-Cr alloys

The level of chromium plays an essential role in irradiation tolerance of Fe-Cr ferritic alloys. However, conflicting results have been reported regarding the dependence of cavity swelling under irradiation on Cr level and temperature. Here, we have performed a comprehensive set of simultaneous dual-ion (Ni + He) irradiations to high dose (~30 displacements per atom, dpa) at 400–550 °C on a series of ultra-high purity Fe and Fe-Cr binary alloys (3–14 wt.%Cr). Helium co-implantation rates of 0.1 and 10 appm He/dpa were selected to examine He synergistic effects relevant for fission and fusion reactor conditions, respectively. Cavities were observed in all irradiated samples by transmission electron microscopy. The results show that higher He implantation rate causes a shift in the swelling peak to higher temperatures in both Fe and Fe-Cr alloys. When assuming smaller cavities as biased sinks, the non-monotonic nature of the cavity swelling behavior is related to the ratio of biased to unbiased point defect sink strengths. Cr-enriched precipitates were observed in Fe-14Cr irradiated at 400 °C by atom probe tomography. Our analysis suggests the formation of Cr-enriched precipitates could suppress cavity swelling for Fe-Cr alloys with Cr content above 10 wt%.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Computer vision models and advanced TEM imaging for microstructures of irradiated AM316 stainless steels

Advancements were made in automating microscopy-based material characterization, particularly in studying irradiation effects on additively manufactured (AM) materials using machine learning (ML) and computer vision (CV). These automation efforts address the challenges of analyzing complex microstructures, accelerating the detection of irradiation-induced defects. Two CV models were developed at Argonne National Laboratory (ANL) to enhance transmission electron microscopy (TEM) analysis of irradiated AM 316 stainless steel. The first model focused on the detection of irradiation-induced dislocation loops, which contribute to material hardening and embrittlement. These loops, categorized as faulted or perfect, were automatically detected and classified using a Mask R-CNN model trained on TEM images from both in-situ and ex-situ ion irradiation experiments. The model achieved high accuracy, with precision, recall, and F1 scores of 0.839, 0.734, and 0.776, respectively, demonstrating its effectiveness in analyzing dislocation loops in irradiated AM materials. The second CV model was developed to analyze the size and wall thickness of dislocation cells in laser powder bed fusion (LPBF) 316 stainless steel. Using a U-Net++ architecture with EfficientNet as the encoder, the model was trained on TEM images to segment and measure cell size and wall thickness.

36 MATERIALS SCIENCE↗