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At least 577 records · Page 32

Development of Binder Jet Compatible Silicon Carbide Mixtures for Increased Sintered Density

Binder jet additive manufacturing can process a variety of ceramic powder feedstocks to manufacture near net shape green parts that are subsequently sintered to achieve densification. In particular, silicon carbide (SiC) is a promising ceramic material for heat exchangers in energy storage applications and binder jet is a well-suited process for manufacturing these heat exchangers due to the often geometrically complex designs. However, the need for good powder flowability in binder jet printing often limits the feedstock powder to be larger particles rather than that of ultra fine submicron powders used in conventional ceramic processing, which are more readily densified during sintering. The present work explores the use of various powder mixtures and sintering settings to identify strategies for achieving high density sintered parts in binder jet compatible systems without the use of infiltration. Liquid-phase sintering additives and bimodal powder mixtures are explored alongside different sintering temperatures, rates, atmospheres, and hold times. Two mixtures were found to be good candidates for further exploration: 1) 90 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 mixture achieved the highest sintered relative density of 91.2%; and 2) a bimodal mixture comprised of 45 wt% 10 µm SiC + 45 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 had the best powder flowability of the powders measured and a 75.1% sintered relative density.

25 ENERGY STORAGE↗

Investigation of Carbide Inclusions in Cast Uranium [Slides]

Outline - Introduction: The motivations for the project, and some background on inclusions in uranium, and about the samples; Lath Inclusion Morphology: Looking at the morphology of a specific family of carbide inclusions in casting 20; Clustering of Lath Inclusions: Investigating the group behavior of these lath shaped inclusions from the inner to outer edges; Conclusions: Final thoughts on the lath inclusions and future work ideas.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Qualification of Commercially Available Silicon Carbide for Passive Thermometry in Reactor Experiments – FY23 Status Report

Silicon carbide (SiC) is often used as a passive temperature indicator for uninstrumented in-core nuclear experiments. For the past several decades, Oak Ridge National Laboratory has relied primarily on SiC thermometry manufactured by Dow Chemical Company, formerly Rohm and Haas because of the material’s high density and reduced grain boundary elements. Although Dow SiC has performed well in this application, this material is no longer commercially available, and a new supplier is needed for future experiments. To determine a suitable replacement, a study was initiated on five types of SiC from four commercial vendors. Several critical properties, including density, electrical resistivity, chemical purity, grain structure, crystal structure, and strength were measured in samples from each material. Additionally, thermometry specimens were manufactured for irradiation in the High Flux Isotope Reactor at nominal temperatures of 300°C, 600°C, and 900°C, which will be measured using continuous dilatometry at a later date. This report provides an update of commercially available SiC material characterization and the irradiation capsule design.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Distributed Temperature Profiles of Silicon Carbide Catalyst Bed in a Microwave Reactor using Fiber-optic Sensor

Microwave heating is of great interest for reducing greenhouse gas emissions of catalytic chemical conversion processes because it can heat up the reactants rapidly and efficiently and accelerate reaction rates. In microwave-assisted catalytic thermochemical conversion processes, accurate internal temperature measurement would help facilitate effective process control. Metallic thermocouples interfere and spark in the microwave heating environment, so they are not an option. Infrared pyrometers typically provide a single temperature value by averaging over a finite surface area of the catalyst bed. In this work, we use fiber-optic sensors passing through the catalyst bed to provide more accurate temperatures along the height of the catalyst bed. The fiber optic sensors are immune to the electromagnetic microwave radiation and provide temperature profiles along their length. Here, custom fiber-optic sensors were coupled to the optical distributed temperature sensing devices to measure the temperature profiles along the height of the catalyst bed at high temperatures with ~1 mm spatial resolution. The sensing devices use optical frequency domain reflectometry (OFDR) technique for distributed temperature measurement. This work shows the temperature profiles along the height of the silicon carbide powder catalyst bed in the variable and fixed frequency microwave reactors.

Thapa, Juddha↗

Lower length scale model for palladium attack of silicon carbide in TRISO fuel

TRistructural ISOtropic (TRISO) particle fuels rely on silicon carbide (SiC) as the primary barrier for metallic fission product (FP) release. Palladium (Pd) generated by fission degrades the SiC layer, resulting in the formation of lamellar layers of palladium silicides (PdxSi) and carbon (C) perpendicular to the direction of attack. The Pd attack has been hypothesized to be responsible for failure of the SiC layer and enhance FP release. To better understand and quantify Pd attack of SiC in TRISO particles, a multiscale, mechanistic model of Pd transport is being developed by the NEAMS program. Previous work provided an initial hypothesis for modeling lamellar microstructure formation in SiC due to Pd attack using a phase-field model. The work described in this report builds on the previous model by using molecular dynamics (MD) simulations to parameterize the phase-field model kinetics, and build a reduced order model in BISON using the improved mesoscale Pd penetration model.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Binder Jet Additive Manufacturing of Silicon Carbide Solar Reactor (CRADA Report)

Achieving high powder packing density is critical in binder jet additive manufacturing (BJAM), as it directly influences the final part density, mechanical properties, and sintering behavior. Multi-modal powder blends, which combine particles of different sizes, have been explored as a strategy to optimize packing efficiency and minimize defects. In this study, bimodal and trimodal powder blends were obtained by mixing silicon carbide powder in three different sizes. These results show that increased powder density is achievable with bimodal powder blends but is reduced in trimodal blends, and it was found that a 13% increase in the powder tap density was achieved using a bimodal blend of powder. The powder size distribution of the bimodal blend was measured at various stages during binder jet additive manufacturing and, no measurable powder separation occurred even after eight prints. Overall, this study shows limited advantage to trimodal powder blends but good promise for trimodal blends for increasing printed density while maintaining reusability in the binder jet process.

99 GENERAL AND MISCELLANEOUS↗

Binder jet additive manufacturing of silicon carbide solar reactor

Achieving high powder packing density is critical in binder jet additive manufacturing (BJAM), as it directly influences the final part density, mechanical properties, and sintering behavior. Multi-modal powder blends, which combine particles of different sizes, have been explored as a strategy to optimize packing efficiency and minimize defects. In this study, bimodal and trimodal powder blends were obtained by mixing silicon carbide powder in three different sizes. These results show that increased powder density is achievable with bimodal powder blends but is reduced in trimodal blends, and it was found that a 13% increase in the powder tap density was achieved using a bimodal blend of powder. The powder size distribution of the bimodal blend was measured at various stages during binder jet additive manufacturing and, no measurable powder separation occurred even after eight prints. Overall, this study shows limited advantage to trimodal powder blends but good promise for trimodal blends for increasing printed density while maintaining reusability in the binder jet process.

36 MATERIALS SCIENCE↗

Automated Segmentation of Twin Boundaries in TRISO Silicon Carbide Using Deep Neural Networks

Coated particle fuels, such as the tristructural isotropic (TRISO) fuel particle, are essential for high-temperature gas reactor (HTGR) applications due to their efficiency and stability under normal and off-normal conditions. However, widespread commercialization and deployment of this technology for next-generation nuclear applications require robust quality assurance and quality control (QA/QC) methods linking fabrication, properties, and performance. Of the many important metrics for TRISO QA/QC, quantification of the silicon carbide (SiC) microstructure is critical because it correlates with fission product retention during irradiation. Previous work has shown extensive twinning of the SiC microstructure, which strongly affects microstructural metrics; however, twin grain boundaries are not expected play a significant role in fission product diffusion. This report summarizes the initial development, training, and testing of a machine learning image processing algorithm to detect twin grain boundaries in a backscattered electron image, which can be removed so that microstructural metrics can be recalculated for legacy data. Further development and deployment of this model will provide automated, scalable improvement of potential QA/QC methods for the SiC layer of TRISO particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Optimization of boron carbide density using direct current sintering for use as sputtering sources at the National Ignition Facility

Several experimental trials were conducted to determine optimal sintering parameters and compositions for purchased boron carbide powder using spark plasma sintering/direct current sintering. Sputtering targets used to create ablators for the National Ignition Facility have been unable to survive post processing procedures suggesting that in-house fabrication may yield better results due to extended control.

36 MATERIALS SCIENCE↗

SILICON CARBIDE THERMOMETRY USING RAMAN SPECTROSCOPY ON IRRADIATED TRISO PARTICLES

Silicon carbide (SiC) passive thermometry has emerged as a promising post-irradiation examination (PIE) technique for estimating irradiation temperature near the end of irradiation. While dilatometry techniques have been traditionally used to analyze prismatic samples after irradiation, Raman spectroscopy has recently been shown to provide comparable results by analyzing Raman-active phonon modes. In this work, Raman spectroscopy has been applied to the SiC layer of cross-sectioned irradiation tristructural isotropic (TRISO) particles from the AGR-5/6/7 experiment to evaluate the feasibility of particle-scale passive thermometry. Two-dimensional Raman mapping was used to measure the position of the SiC longitudinal optical (LO) phonon, which was then converted to an apparent irradiation temperature using a previously established empirical correlation. Particles from AGR-5/6/7 Compacts 2-2-1 and 5-1-3 were selected as their calculated time-averaged, volume-averaged (TAVA) temperatures (828°C and 706°C, respectively) fall within the range of the sensitivity of the experimental approach. The use of SiC thermometry was anticipated to confirm or highlight potential deviations from calculated end-of-life TAVA temperature across compacts. Four particles from Compact 2-2-1 and two particles from Compact 5-1-3 were selected based on 110mAg inventory (either some measurable activity or below the minimum detection limit) which is commonly used as an indicator of in-pile temperature variation of particles within the same compact. Across every particle selected it was determined that the average LO peak position was located around 968 cm-1 to 969 cm-1. Using the previously determined empirical correlation, this corresponds to an irradiation temperature around 950°C to 966°C, which does not align with the reported TAVA temperature values. This discrepancy in apparent irradiation temperatures likely reflects a combination of uncertainties in the calculated particle temperatures and differences in irradiation history between the present specimens and those used to establish the empirical Raman calibration such as neutron flux (damage rate) and SiC microstructure (as fabricated and irradiated).

Vawdrey, Josh [ORNL]↗

Raman spectroscopy of neutron irradiated silicon carbide

The effects of neutron irradiation on microstructural evolution and the resultant changes in physical and mechanical properties are of critical importance for the development of silicon carbide (SiC) materials for nuclear applications. This study neutron-irradiated βSiC under a wide range of conditions at temperatures between 235 and 750°C and neutron doses of 0.01–11.8 displacements per atom, and then evaluated the effects on the SiC structure using Raman spectroscopy. The SiC optical phonon lines were shifted to lower wavenumbers by irradiation. Correlations were found among the wavenumber of the longitudinal optical phonon line, irradiation-induced swelling, and irradiation temperature. The peak shift also correlated indirectly with decreasing thermal conductivity of irradiated SiC. The irradiation-induced peak shift is explained by combinations of lattice strain, reduction of the elastic modulus, and other factors including decreasing coherent domain size. These findings bridge irradiation-induced microstructural changes and property changes and illustrate how Raman spectroscopy is a useful tool for nondestructively assessing irradiated SiC materials for nuclear applications.

Koyanagi, T.↗