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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7

Precision Local Burnup Assessment Through Dynamic Peak Fitting in Atom Probe Tomography for Depleted, Enriched, and Irradiated Metallic and Ceramic Fuels

Abstract Burnup estimation in nuclear fuels is vital for evaluating fuel performance, transportation, and safe fuel storage. Accurate assessments of burnup from service period and spent fuels involve tracking the consumption of fissile isotopes of uranium (U) offering a direct insight into energy changes within the fuels especially for thermal spectrum reactors. In current approach, mass spectroscopic technique in atom probe tomography (APT) is utilized for accurate quantification of U isotopes. Quantification of U peaks in mass spectrum is performed on asymmetric shapes due to delayed signals, known as thermal tails, particularly for poorly conducting samples analyzed in laser mode. In this study, we introduce a novel quantification tool for isotopic analysis from APT datasets by developing a fitting algorithm based on shapes of the peaks. A MATLAB-based dynamic peak fitting toolbox is developed and designed to adapt to various peak shapes, ensuring accurate quantification of U isotopes. The effectiveness of this approach is demonstrated in standard Ni-Cr sample, depleted and enriched U samples, and U-based fuels with different burnup levels. The viability of this approach for isotopic quantification is demonstrated on both metallic and ceramic fuels.

Burnup↗

Smaller feature size impairs densification in digital light processing 3D printed ceramic samples

In this study, we investigate how geometric miniaturization affects the sintering densification behavior of alumina cylinders with various wall thicknesses (down to ∼500 µm in green body) fabricated via digital light processing (DLP). As the wall thickness decreased, the density of the sintered samples consistently declined. Microstructural characterization revealed the presence of a crack-rich surface skin that is ∼500 µm thick. As the wall thickness decreases, the skin's volume fraction rises, and its poor local densification increasingly dominates the part average, leading to an overall decrease in the density of the sintered samples. For the thinnest wall (500 µm) cylinder, macroscopic warping occurred during sintering. We suggest that warping further disrupts particle packing and induces through-thickness nonuniformity, further impairing densification in addition to the skin-fraction effect. These results highlight how geometric miniaturization may adversely influence the sintering behavior and final density of DLP-printed ceramics through distinct densification-limiting mechanisms.

Materials science↗

A comparison of ceramic and carbon-based reductants for vitrification of low-activity waste

Sucrose is the current baseline additive at the Hanford Waste Treatment and Immobilization Plant in Washington, USA to control foaming during waste feed to glass transitions and the redox state of the glass melt. Alternative reductants are being investigated to alleviate strain on effluent treatment from toxic acetonitrile production from incomplete combustion of sucrose. This study evaluates ceramic additive options including B4C, B6Si, SiC and VB2 in simulated low-activity waste feed, as well as coke dust, probing the feed volume expansion during melting as well as the gas evolution. All alternative reductant options examined significantly reduced acetonitrile production, however there was variability in their effectiveness as foam-reducing agents. VB2 and coke at the appropriate ratios were similarly effective as sucrose in controlling both foam volume and glass redox state, but with considerably less acetonitrile production. B4C, B6Si and SiC showed more promising foam control and very little acetonitrile production, however all of the final glasses were over reduced, i.e., Fe2+/FeT = 0.5. These alternative reductant studies provide operational flexibility to the operation of the vitrification plant, as well as options for alternative raw materials in industrial glass melting.

Rigby, Jessica C. (ORCID:0000000235719977)↗

Orientation microscopy–assisted grain boundary analysis for protonic ceramic cell electrolytes

Abstract Grain boundaries in protonic ceramic cell (PCC) electrolytes hinder proton transport, reducing interfacial conductivity. In multicomponent PCC electrolytes, the inclusion of sintering aids further accentuates the complexity of grain boundaries. In this study, we synthesize nanocrystalline BaCe 0.4 Zr 0.4 Y 0.1 Yb 0.1 O 3− δ thin films via pulsed laser deposition and analyze their grain boundary character distributions using orientation data collected by precession electron diffraction technique. The results reveal an anisotropic distribution of grain boundary characters, with notably high populations of 180°‐tilt and twist grain boundaries. These findings provide critical insights into identifying the predominant grain boundaries in this PCC electrolyte material, assessing the vast five‐dimensional grain boundary space.

Patel, Sooraj [School of Aerospace and Mechanical ↗

A new method for measuring refractory corrosion of ceramics in glass

Abstract Nuclear waste glass vitrification furnaces are lined with refractory ceramic blocks to contain the molten glass. The refractory liner is susceptible to corrosion and has a finite service lifetime. For this reason, predicting the refractory corrosion in contact with molten glass is integral to estimating melter service lifetime. Standardized laboratory tests varying time and temperature are commonly performed to estimate refractory material loss as a function of glass composition. These data are time and resource‐intensive to collect and are susceptible to considerable measurement error. In order to accelerate glass formulation and design for nuclear waste vitrification, methods are needed to increase laboratory‐scale throughput while maintaining data quality. In this work, a method to remove the residual glass from a corroded coupon using hydrofluoric acid is presented that accelerates the throughput of sample analysis while simultaneously facilitating more accurate measurements.

Amoroso, Jake W. [Savannah River National Laborato↗

Ink-sprayed transparent ceramic multilayer planar waveguides for ribbon lasers

Multilayer transparent ceramic planar waveguides were fabricated using a newly developed particle-loaded ink spraying method, characterized, and lased. Waveguides with five Yb:YAG gain regions and four Lu:YAG index-matched regions were produced for application as a “ribbon laser,” as well as a homogeneous Yb:YAG waveguide. Elemental mapping revealed that the waveguide thicknesses varied from 40 to 69 μm, comprised of layers of less than 10 µm. The Yb concentration profiles were fit to a diffusion profile. The homogeneous and multilayer waveguides were tested in a laser cavity and produced similar slope efficiencies, with a maximum of 31% achieved. In conclusion, their beam profiles provided evidence of the ribbon structure affecting the preferred mode.

Osborne, Ross [Lawrence Livermore National Laborat↗

Small-scale Assessment of Simplified Ceramic Waste Form Processing

The feasibility of directly processing glass-bonded sodalite ceramic waste form materials by heating a mixture of Zeolite 4A, chloride salt, and sodium borosilicate binder glass was demonstrated by generating laboratory-scale materials. This direct processing method eliminates pre-setting the moisture content of the Zeolite 4A, eliminates the step of occluding salt in the prepared Zeolite 4A prior to processing, and can be conducted using larger particle sizes of crushed Zeolite 4A and crushed borosilicate glass than those called for in the current method. These simplifications are expected to facilitate material transfer and handling in a hot cell or controlled atmosphere environment and be more readily implemented at large scale than the current method. Most materials made to assess these simplifications were directly processed at 925 °C for two hours in an argon atmosphere glovebox, but one material was processed at 925 °C for four hours and one material was processed at 880 °C for two hours. Sodalite was generated and became microencapsulated by the binder glass in all materials. The microstructures were uniform throughout each product, were similar in all products, and were similar to the microstructures of materials made previously using the pressureless consolidation or hot isostatic pressing methods. Various formulations showed the efficiency of sodalite generation was not sensitive to the salt-to-Zeolite 4A ratio or salt-to-glass mass ratio, although a greater relative mass of glass is required to encapsulate sodalite generated from large particles of aggregated Zeolite 4A. The upper limit of salt loadings that can be effectively processed remains to be determined. The effectiveness of direct processing provided new insights into the conversion mechanism. The salt was likely dissolved into the glass that transported NaCl into the Zeolite 4A aggregates and sodalite was generated in situ as NaCl migrated from the outside of the aggregate inward. Other salt cations (e.g., potassium, strontium, cesium, and probably lithium) remain dissolved in the glass encapsulating the zeolite/sodalite domains. When the glass solidifies during cooling, small halite inclusion phases form in glass within sodalite domains and large mixed salt inclusions form in glass surrounding the sodalite due to the low solubility of chloride in the (solid) glass. Other salt cations were oxidized during processing and formed inclusions in the bulk glass (e.g., neodymium). Initial degradation tests show the dissolution behavior of directly processed CWF (SCWF) materials is similar to CWF materials made using different methods.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Methanol from Integrated Direct Air Capture and Ceramic Electrolysis (MIDACE)

The Methanol from Integrated Direct Air Capture and Ceramic Electrolysis (MIDACE) project advanced a novel system concept for integrating pressurized co-electrolysis of steam and crude carbon dioxide captured directly from ambient air using a sorbent technology. The co-electrolysis produced syngas provides feedstock for a gas-to-liquid methanol synthesis reactor. The system recovers waste heat from the reactor and electrolyzer into regenerating the direct air capture sorbent. The purpose of the project was to demonstrate critical integration elements of the design and perform a technical study illustrating how a large-scale installation could achieve the $800/ton program target for green methanol production. The concept addresses the program objective to consolidate operations by combining crude CO 2 cleanup, hydrogen production, and partial CO 2 reduction steps within a carbon tolerant high temperature electrolyzer. The design lowers costs by simplifying the methanol recovery cycle, reducing carbon losses from venting, reducing sensitivity to catalyst selectivity, and avoiding syngas compression.

10 SYNTHETIC FUELS↗

Enhancing 300 Degree Celsius Electronic Packaging with Ceramic PCBs and Advanced Interconnection Techniques

Geothermal energy development requires downhole tools that operate reliably at temperatures up to 320 °C. While MWD tools work without thermal protection and logging tools use vacuum flasks for limited high-temperature use, Sandia National Laboratories is developing durable electronics on ceramic PCBs with protective coatings to enable long-term operation of geothermal instruments at sustained temperatures up to 300 °C.

Wright, Andrew Alexander [Sandia National Laborato↗

PIP-II SRF Couplers Fabrication Status and Addressing Ceramic Yield Challenges

The PIP-II project requires reliable SRF couplers to deliver high RF power to the cavities. This talk presents the current status of coupler fabrication, including progress on procurement, assembly, and testing. In particular, it focuses on the challenges encountered with ceramic window production, where limited yield has become a concern. Observed issues and inspection results will be discussed, together with the actions taken to improve quality and consistency. The path forward, including ongoing work with vendors and process adjustments, will also be outlined.

Aiazzi, Tommaso [Fermilab] (ORCID:0009000297503407↗

Control of wetting and uniformity via ZrSi x formation in ceramic-to-metal joints fabricated using Ag-Zr brazes

The deposition of a 2.0 µm SiO 2 film on the alumina surface in Kovar TM /94% alumina joints enables the formation of a silicide reaction layer on the alumina during brazing with 97Ag2Zr1Cu. Additionally, the average and standard deviation of joint thickness decrease from 50 to 15 and 29 to 4 µm, respectively compared to joints without added SiO 2 . Finally, the average failure stress of these braze joints was 45 MPa, while that of similar joints without added SiO 2 was 90 MPa. Sessile drop experiments of 98Ag2Zr on SiO 2 and 99.6% Al 2 O 3 substrates show that the braze wets and spreads to 3x its original area on SiO 2 with a wetting angle near 0°, but remains the same area on 99.6% Al 2 O 3 with a wetting angle of 106.6°. Focused-ion-beam scanning electron microscopy analysis of a cross-section of the 98Ag2Zr sessile drop on the SiO 2 substrate has shown that Zr reacts with SiO 2 to form Zr oxide and silicide layers. Scanning transmission electron microscopy diffraction and energy dispersive X-ray spectroscopy analysis indicate this silicide layer contains tetragonal Zr 5 Si 4 . In conclusion, analysis shows the silicide layer enhances wetting and joint uniformity while unreacted SiO 2 embrittles the joint and degrades strength.

alumina↗

Spatially Resolved Raman Spectroscopy of Thin Carbon Interphase in SiC Ceramic Matrix Composites

A dedicated analysis method is presented to extract the Raman spectrum of an interphase layer thinner than the laser spot size. We focused on spatial correlations between the contrast of optical micrographs and Raman hyperspectral data to predict the constituents of the mixed spectra measured near the interphase. By employing a mapping step size of 0.1 μm, the Raman spectrum of approximately 0.3-μm-thick carbon interphase in a SiC fiber-reinforced SiC matrix composite was extracted from data acquired with a theoretical spot size of about 0.7 μm. Notably, conventional chemometrics procedures were unable to isolate the interphase signal, instead producing a spectrum representing a mixture of interphase and matrix. This study used another composite with approximately 0.9-μm-thick interphase to validate the analysis method, enabling direct measurement of the interphase spectrum. The proposed Raman analysis method has advantages in specimen volume and turnaround time compared to traditional characterization methods, such as transmission electron microscopy. In conclusion, this study also evaluates the applicability of the analysis method to different composite materials and identifies key requirements of the measurements, including the ratio of interphase thickness to spot size and the homogeneity of the surrounding matrix.

ceramic matrix composite↗

Fast ionic conduction achieved through the design and synthesis of ceramic heterointerfaces

Lithium (Li) chloride and iron oxychloride (FeOCl), typically nonconductive, were combined to form a [Li 1+δ Cl] δ+ /[FeOCl] δ- heterointerface composite material (LFH), achieving ionic conductivities of >1 mS cm -1 . Analysis techniques (scanning transmission electron microscopy [STEM] and electron energy-loss spectroscopy [EELS]) indicated that the microstructure of LFH consisted of an amorphous LiCl-based shell surrounding a crystalline FeOCl-based core. Electrochemical measurements alongside solid-state 6,7 Li nuclear magnetic resonance (NMR) and molecular dynamic simulations revealed Li+ as the sole conductive species, with a diffusion barrier of ~0.25 eV. X-ray photoelectron spectroscopy (XPS) and X-ray absorption fine structure (XAFS) results further supported interstitial Li + diffusion at the heterointerface and within the LiCl phase, made possible by the heterointerface. Despite susceptibility to electronic conductivity, iron’s defects and multivalency (Fe³⁺, Fe²⁺) enable the Fe–O–Cl framework to accept Cl - , facilitating Li⁺ ionic conduction. Finally, a prototype solid-state cell (showing 97% Coulombic efficiency) demonstrated the viability of this heterointerface design for applications in energy storage.

36 MATERIALS SCIENCE↗

Selective laser sintering and spark plasma sintering of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide ceramics

Abstract Two advanced manufacturing processes, spark plasma sintering (SPS) and selective laser sintering (SLS), have been developed for synthesis of (Zr,Nb,Ta,Ti,W)C compositionally complex carbide (CCC) via reactive sintering of a powder mixture of constitute monocarbides. X‐ray diffraction analysis confirmed that the single‐phase CCC can be formed by both SPS and SLS. While a homogenous microstructure with uniform metal element distributions was developed during SPS, three‐layer microstructures with a thin TiC‐rich layer and two TaC‐rich layers along with a TiO 2 ‐rich surface layer containing W nanoparticles were formed during SLS. In addition, cellular structures with W, Zr, and Ti element segregation and dislocations on cell boundaries were observed in the SLS‐CCC sample, indicating the effect of nonequilibrium conditions on microstructure formation during laser melting followed by rapid cooling and solidification process. Compared to the SPS‐CCC sample, the SLS‐CCC showed enhanced hardness and reduced thermal conductivity, which may be related to their unique cellular structures.

36 MATERIALS SCIENCE↗

Coal-Waste-Enhanced Filaments for Additive Manufacturing of High-Temperature Plastics and Ceramic Composites

In the United States, coal waste from over a century of mining and burning coal for heat and electricity has accumulated as mountains of coal fly ash and bottom ash and acre-size ponds, coal fines and gob. These materials can be a problem for local communities and water systems. A cost-effective process to utilize high volumes of these coal wastes in a high-value product would be beneficial to those communities by reducing the amount of waste and providing jobs, manufacturing components, and materials from the waste. Many coal-to-products technologies (e.g., carbon fibers, graphene, carbon foam) rely on carefully choosing the starting material and then altering it chemically or thermally to make the products work. Due to the wide variability of composition and coal content in typical coal waste streams, many high-volume coal waste streams are likely to be unsuitable for use in those technologies. Semplastics’ technology has been shown to utilize most types of coal waste successfully without any pre-selection or pre-processing requirements other than a nominal particle-size reduction for wastes like bottom ash. This characteristic of Semplastics’ solution may enable the use of much larger volumes of a wider range of coal wastes than other coal-to-products technologies. In this project, Semplastics leveraged its unique experience with both coal waste (fly ash or coal combustion residuals), resin materials, and 3D printing to develop 3D printer filaments using common coal wastes – bituminous coal fines and fly ash – and researched the feasibility of using other forms of coal waste as fillers. Simple 3D-printed parts were successfully produced from the coal waste enhanced filaments, which were found to have improved strength and stiffness.

01 COAL, LIGNITE, AND PEAT↗