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At least 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

TEX-Chlorine Assemblies: Highly Enriched Uranium Plates with Sodium Chloride Absorbers Using Polyethylene Moderator and Polyethylene Reflector

This evaluation documents highly enriched uranium (HEU) experimental critical configurations with polyethylene moderators and sodium chloride absorbers conducted as part of the United States Nuclear Criticality Safety Program’s Thermal/Epithermal eXperiments (TEX) program. HEU-MET-MIXED-021 provides the benchmark evaluation of five TEX experiments designed to establish baseline configurations with HEU Jemima plates moderated by high density polyethylene (HDPE). The TEX-HEU experiments were designed to cover five different fission energy regimes by varying the thickness of the interstitial HDPE moderator, with varying fractions of thermal, intermediate, and fast fissions, and to be easily modified to accommodate test materials of interest. HEU-MET-INTER-013 documents the first TEX-HEU variation, incorporating hafnium in seven different experimental configurations. This evaluation covers an additional variant that incorporates absorber plates of compacted high-purity sodium chloride salt. These experiments were motivated by a criticality safety need for validation data for uranium purification by means of electrorefining with chloride salts, especially thermal and intermediate energy configurations resulting from moderator upset conditions, and their design was optimized by matching sensitivity profiles from application cases. All three experimental configurations are judged to be acceptable as benchmark cases. The main parameter varied between the configurations is the thickness of the polyethylene moderators and the sodium chloride absorbers between the HEU plates. Varying the thickness of the polyethylene tunes the neutron energy spectrum between majority thermal (Case 1 and 2) and intermediate (Case 3). The fission fractions, presented in Table 1, are determined calculationally. Case 3 is cross listed as HEU-MET-INTER-014.

42 ENGINEERING↗
DOE OSTI2020

Erratum to: Soft- and reactive landing of ions onto surfaces: concepts and applications

Soft- and reactive landing of mass-selected ions is gaining attention as a promising approach for the precisely-controlled preparation of materials on surfaces that are not amenable to deposition using conventional methods. A broad range of ionization sources and mass filters are available that make ion soft-landing a versatile tool for surface modification using beams of hyperthermal (<100?eV) ions. The ability to select the mass-to-charge ratio of the ion, its kinetic energy and charge state, along with precise control of the size, shape, and position of the ion beam on the deposition target distinguishes ion soft landing from other surface modification techniques. Soft- and reactive landing have been used to prepare interfaces for practical applications as well as precisely-defined model surfaces for fundamental investigations in chemistry, physics, and materials science. For instance, soft- and reactive landing have been applied to study the surface chemistry of ions isolated in the gas-phase, prepare arrays of proteins for high-throughput biological screening, produce novel carbon-based and polymer materials, enrich the secondary structure of peptides and the chirality of organic molecules, immobilize electrochemically-active proteins and organometallics on electrodes, create thin films of complex molecules, and immobilize catalytically active organometallics as well as ligated metal clusters. In addition, soft landing has enabled investigation of the size-dependent behavior of bare metal clusters in the critical subnanometer size regime where chemical and physical properties do not scale predictably with size. The morphology, aggregation, and immobilization of larger bare metal nanoparticles, which are directly relevant to the design of catalysts as well as improved memory and electronic devices, have also been studied using ion soft landing. This review article begins in section 1 with a brief introduction to the existing applications of ion soft- and reactive landing. Section 2 provides an overview of the ionization sources and mass filters that have been used to date for soft landing of mass-selected ions. A discussion of the competing processes that occur during ion deposition as well as the types of ions and surfaces that have been investigated follows in section 3. Section 4 discusses the physical phenomena that occur during and after ion soft landing, including retention and reduction of ionic charge along with factors that impact the efficiency of ion deposition. The influence of soft landing on the secondary structure and biological activity of complex ions is addressed in section 5. Lastly, an overview of the structure and mobility as well as the catalytic, optical, magnetic, and redox properties of bare ionic clusters and nanoparticles deposited onto surfaces is presented in section 6. © 2015 Wiley Periodicals, Inc. Mass Spec Rev 35:439–479, 2016.

Johnson, Grant E.↗
DOE OSTI2023

Enhanced rare-earth separation with a metal-sensitive lanmodulin dimer

Technologically critical rare-earth elements are notoriously difficult to separate, owing to their subtle differences in ionic radius and coordination number. The natural lanthanide-binding protein lanmodulin (LanM) is a sustainable alternative to conventional solvent-extraction-based separation. Here we characterize a new LanM, from Hansschlegelia quercus (Hans-LanM), with an oligomeric state sensitive to rare-earth ionic radius, the lanthanum(III)-induced dimer being >100-fold tighter than the dysprosium(III)-induced dimer. X-ray crystal structures illustrate how picometre-scale differences in radius between lanthanum(III) and dysprosium(III) are propagated to Hans-LanM’s quaternary structure through a carboxylate shift that rearranges a second-sphere hydrogen-bonding network. Comparison to the prototypal LanM from Methylorubrum extorquens reveals distinct metal coordination strategies, rationalizing Hans-LanM’s greater selectivity within the rare-earth elements. Finally, structure-guided mutagenesis of a key residue at the Hans-LanM dimer interface modulates dimerization in solution and enables single-stage, column-based separation of a neodymium(III)/dysprosium(III) mixture to >98% individual element purities. This work showcases the natural diversity of selective lanthanide recognition motifs, and it reveals rare-earth-sensitive dimerization as a biological principle by which to tune the performance of biomolecule-based separation processes.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Polymer Tacticity Effects in Polymer–Lanthanide Chelation Thermodynamics

Metal-chelating polymers are critical components in numerous applications. However, despite the known influence of polymer tacticity on both bulk and solution properties, most materials used in metal-chelation applications are atactic. Here, we investigate the relationship between polymer tacticity and polymer–lanthanide interactions in aqueous solution. We synthesized a series of five poly(methacrylic acid)s with systematic variations in tacticity (20–99% m diads) and used isothermal titration calorimetry to measure the thermodynamics of lanthanide binding to each material (ΔH, ΔG, ΔS, K a , and stoichiometry). We observed enthalpy–entropy compensation across this tacticity series, finding that both |ΔH| and |ΔS| decreased with decreasing m diad content while ΔG remained similar. Molecular dynamics simulations of the polymer–metal interactions revealed that the observed differences in binding thermodynamics may be largely ascribed to differences in polymer flexibility. Furthermore, these combined experimental and computational results demonstrate that metal binding can be influenced by altering the polymer stereochemistry, ultimately influencing the design of more efficient metal-chelating materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Theory of the strange metal Sr 3 Ru 2 O 7

The bilayer perovskite Sr 3 Ru 2 O 7 has been widely studied as a canonical strange metal. It exhibits T -linear resistivity and a T log(1/ T ) electronic specific heat in a field-tuned quantum cr itical fan. Criticality is known to occur in “hot” Fermi pockets with a high density of states close to the Fermi energy. We show that while these hot pockets occupy a small fraction of the Brillouin zone, they are responsible for the anomalous transport and thermodynamics of the material. Specifically, a scattering process in which two electrons from the large, “cold” Fermi surfaces scatter into one hot and one cold electron renders the ostensibly noncritical cold fermions a marginal Fermi liquid. From this fact the transport and thermodynamic phase diagram is reproduced in detail. To conclude, we show that the same scattering mechanism into hot electrons that are instead localized near a 2D van Hove singularity explains theanomalous transport observed in strained Sr 2 RuO 4 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

Physical, Chemical, and Mineralogical Characterizations of MSWI Ash Product and Recommendations for Downstream Processing

The primary objectives of this project are to (1) systematically characterize MSWI ash, and (2) based on characterization findings, design preliminary flowsheets for downstream processing. To achieve these objectives, a total of ten tasks were completed, including sample collection, physical separation tests, liberation tests, synthetic MSWI ash preparation, elemental composition analysis, sequential chemical extraction, mineralogical characterization, pozzolanic activity characterization, thermal stability characterization, processing flowsheet design, TEA and T2M, and project performance reporting. Many useful findings and conclusions were obtained from the exhaustive efforts of this project from several different aspects, including: a) Valuable Metals in MSWI Ash: MSWI ash contains a diverse array of valuable metals. Based on potential recoverable values, the most valuable metals present in MSWI ash include Fe, Ti, Mn, Cu, Zn, V, Co, Ni, Sr, Sn, Ag, Mo, and Sc. Some of these metals have been identified as critical minerals by DOE and DOI, suggesting that MSWI is a promising feedstock for critical mineral recovery. Noticeable graphical and seasonable variations in the valuable metal content of MSWI ash were observed. Nevertheless, it was challenging to discern any clear, definitive patterns for conclusions from those observations. Compared with bottom ash, fly ash contains more volatile metals, such as Zn and Sn, but less nonvolatile metals, such as Fe, Mn, Cu, Zn, Co, and Ni. Mineralogical analyses showed that MSWI ash contains a substantial amount of calcium minerals, such as portlandite, lime, gypsum, and calcite. In addition, it was found that different types of valuable metals often exist in the same particles. b) Physical Separation of MSWI Ash: Both dry sieving and wet sieving were performed on MSWI ash. A notable disparity in the size distribution of the same material was observed when using the two different sieving methods. The disparity is due to the agglomeration of small particles. For the valuable metals investigated, no significant enrichment in a specific size fraction was observed, suggesting that it is challenging to preconcentrate the valuable metals through size fractionation. Due to the presence of ferromagnetic materials, such as Fe, most of the materials reported to the magnetic products obtained by dry magnetic separation. However, the enrichment effect is minimal due to the existence of particle agglomerates. Density separation at a cut-off density of 2.7 SG or higher led to noticeable enrichment of selected valuable metals, particularly Ti. The unburned carbon present in MSWI ash was effectively removed by flotation using diesel as the collector. A novel reagent scheme, Na2S plus cationic collectors, that can efficiently beneficiate nonferrous metals plus Co was developed. c) Liberation Tests: The particle size of MSWI ash was effectively reduced by grinding, and as a result, the encapsulated valuable metal particles (if any) were liberated to a certain degree. However, particle size reductions did not noticeably enhance the beneficiation performance using the physical separation methods, primarily due to the inefficiency of these methods in processing fine particles and/or a possibility that insufficient liberation is not a limiting factor for achieving satisfactory physical separation performance. Valuable metals were classified into water leachable, ion-exchangeable, acid soluble, reducible, oxidable, and insoluble forms. It was found that the distributions in the different categories, i.e., the occurrence modes of the valuable metals, were not affected by the particle size. d) Leaching Characteristics of Metals from MSWI Ash: Most of the valuable metals were extracted from the fly ash samples when using 1 M HCl or HNO3 as the lixiviant. The leaching reaction is a very fast process, which can reach equilibrium within the first 5 min. The releasing of Co, Ni and Ag are sensitive to leaching temperature, a higher recovery value could be obtained when using relatively higher leaching temperatures. The leachability of the valuable metals present in MSWI bottom ash is relatively lower than that of fly ash. Leaching recoveries increased with elevations in the acid concentration. Relatively high leaching recoveries were obtained for REEs, Mn, Co, Ni, Cu, and Zn using 1 M HCl or HNO3 as the lixiviant. Elevations in the reaction temperature noticeably increased the leachability of the valuable metals, whereas the leachability was barely influenced by oxidizing and reducing agents. Similar to fly ash, leaching valuable metals from bottom ash is a rapid process, with most of the leaching reaction completed within the first 5 minutes. e) Combusted iPhones: The original structure of iPhones was remained after treating at 400 ºC and 600 ºC, while after being treated at 800℃, the screen bent, and the back cover of iPhone melted. Increasing the combustion temperature to 1000℃, the screen scattered, and most of the components turned into ashes. Combustion enhanced the leachability of REEs, while the leachability of the other valuable metals, except for Zn, was barely affected. Most of the REEs present in the original iPhones occurred as oxidizable forms. With elevations in the combustion temperature up to 600 ºC, the oxidizable REEs were transformed to acid soluble forms. However, further elevations in temperature resulted in decreases in the acid soluble fraction and corresponding increases in the reducible and oxidizable forms. Additionally, combustion temperature also significantly altered the occurrence modes of other metals present in the iPhones. f) Synthetic MSWI Ash: It was found that in the absence of hydrogen peroxide, all the elements except for Si were leached to certain degrees. It is noteworthy that approximately 80% of Zn was leached with 1.2 M HCl. When hydrogen peroxide was added to the reaction system, noticeable increases in the leaching recovery of Fe, Mn, Co, Ni, and Cu were observed. The leaching recovery of Al and Si was barely affected by adding hydrogen peroxide. These results suggested that the majority of Zn in the synthetic MSWI ash existed as metal oxide, a portion of Fe, Mn, Co, Ni, and Cu existed as metal oxide, and Al and Si are associated with glasses which are difficult to leach. Additionally, the remaining Fe, Mn, Co, Ni, and Cu in the metallic form were efficiently oxidized in the presence of hydrogen peroxide. g) Pozzolanic Activity and Thermal Stability of MSWI Ash: MSWI fly ash has higher pozzolanic activity compared to the bottom ash sample, which indicates that the fly ash sample consumed more portlandite because of its smaller particle size as reactivity fundamentally relates to reaction surface area. However, after the recovery of valuable elements, the pozzolanic activity of both the valuable elements fraction and the less valuable elements-rich products decreased significantly, which means that the valuable elements recovery lowers the Ca(OH)2 consumption, thus leading to the low activity of SCM. h) Flowsheet Design for Metal Recovery from MSWI Ash: Based on the results of the comprehensive physical separation and acid leaching tests, circuits that enable the beneficiation of the valuable metals were developed. In these circuits, the valuable metals are recovered into nonferrous, ferrous, and other valuable metal concentrates, which are processed separately in the acid leaching step. The subsequent separation and purification steps are simplified due to the physical beneficiation step. In addition, the overall recovery cost is reduced since physical beneficiation is much cheaper compared with chemical processing. Using different technologies, such as selective precipitation and solvent extraction, a comprehensive hydrometallurgical circuit was designed, and compounds of Cu, Zn, Mn, Co, and Ni with a purity close to or even higher than 95% were successfully generated.

36 MATERIALS SCIENCE↗
NASA NTRS2008

Deconvoluting the Friction Stir Weld Process for Optimizing Welds

In the friction stir welding process, the rotating surfaces of the pin and shoulder contact the weld metal and force a rotational flow within the weld metal. Heat, generated by the metal deformation as well as frictional slippage with the contact surface, softens the metal and makes it easier to deform. As in any thermo-mechanical processing of metal, the flow conditions are critical to the quality of the weld. For example, extrusion of metal from under the shoulder of an excessively hot weld may relax local pressure and result in wormhole defects. The trace of the weld joint in the wake of the weld may vary geometrically depending upon the flow streamlines around the tool with some geometry more vulnerable to loss of strength from joint contamination than others. The material flow path around the tool cannot be seen in real time during the weld. By using analytical "tools" based upon the principles of mathematics and physics, a weld model can be created to compute features that can be observed. By comparing the computed observations with actual data, the weld model can be validated or adjusted to get better agreement. Inputs to the model to predict weld structures and properties include: hot working properties ofthe metal, pin tool geometry, travel rate, rotation and plunge force. Since metals record their prior hot working history, the hot working conditions imparted during FSW can be quantified by interpreting the final microstructure. Variations in texture and grain size result from variations in the strain accommodated at a given strain rate and temperature. Microstructural data from a variety of FSWs has been correlated with prior marker studies to contribute to our understanding of the FSW process. Once this stage is reached, the weld modeling process can save significant development costs by reducing costly trial-and-error approaches to obtaining quality welds.

Schneider, Judy↗
DOE OSTI2022

Supramolecular Control of Redox-Mediated Interactions for Ion-Selective Electroseparations

This report summarizes efforts from the Su Group at the University of Illinois at Urbana-Champaign in researching and developing materials and processes for the recovery of rare earth elements and other metal elements that are critical to the United States economy and national security, under DOE Award No. DE-SC0021409. This report highlights efforts in the recovery of: • Transition metal elements (including arsenic, chromium, molybdenum, rhenium, vanadium): Redox-active metallopolymers are able to capture these elements in their oxyanion form. Direct control of target ion capture/release through electrochemical-mediated switching of metallocene binding sites reduces chemical input and lowers generation of waste in element recovery processes. We study the effects of metallopolymer structure on targeted ion binding through a combination of experimental screening of ion selectivity from multi-component mixtures, computational efforts which elucidate the charge-transfer origins of metallocene binding and provide insight on how binding site structure influences selectivity, and state-of-the-art neutron reflectivity of metallocene polymer films to understand the interplay of polymer-ion (charge-transfer), polymer-solvent (polymer hydrophilicity/hydrophobicity), and ion-solvent (ion hydration) interactions with spatial resolution of polymer films. • Rare earth elements (including yttrium, neodymium, europium, gadolinium, dysprosium, cerium): Here we employ redox-copolymers for recovery of rare earth elements by electrochemically regenerated ion-exchange. Rare earth elements require an alternative route to capture/release than directly with metallopolymers since rare earth elements typically exist in cationic form in water. To address this, copolymerization of traditional ion-exchange moieties with metallocene moieties allowed for capture of rare earth elements with the ion-exchange moieties and electrochemical-mediated release of rare earth elements through oxidation of metallocene moieties.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Catalytic Hydrogenation of a Ruthenium Carbonyl to Formyl Enabled by Metal–Ligand Cooperation

Metal formyl complexes are critical intermediates in the reduction of CO to valuable products such as methanol and higher alcohols/hydrocarbons, yet examples of formyl generation via the catalytic hydrogenation of transition metal carbonyl complexes under mild conditions are lacking. The catalytic hydrogenation of a ruthenium carbonyl complex with H 2 to produce a formyl complex is reported here. Two classes of hydrogenation catalysts were compared: bis(diphosphine)-ligated complexes that proceed via termolecular H 2 splitting with an external base and pincer-ligated complexes that proceed via an H 2 splitting mechanism involving metal–ligand cooperativity. The hydride transfer and H 2 splitting steps were evaluated for both classes of catalysts, revealing advantages for catalysts that utilize metal–ligand cooperativity and elucidating conditions to promote formyl generation. Only the pincer-ligated Ir and Ru complexes capable of reacting via pathways involving metal–ligand cooperativity were suitable for catalysis. Using 1–10 mol % of the catalysts (PNP)Ir(H) 2 and (HPNP)Ru(H) 2 (CO) (PNP = ( i Pr 2 PC 2 H 4 ) 2 N – ), which use metal–ligand cooperation to activate H 2 , up to 10 turnovers or up to 71% yield were achieved for the conversion of [Ru(bpy) 2 (CO) 2 ] 2+ (bpy = 2,2′-bipyridine) to the formyl complex [Ru(bpy) 2 (CO)(CHO)] + . The Lewis acid B(C 6 F 5 ) 3 was required as an additive to achieve high yields of the formyl complex using (HPNP)Ru(H) 2 (CO) as a catalyst. In conclusion, the catalytic route avoids the use of expensive stoichiometric reagents, such as borohydride, instead generating metal formyls that are key intermediates in CO reduction schemes with H 2 gas.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1972

The kinetic and mechanical aspects of hydrogen-induced failure in metals

Premature hydrogen-induced failure observed to occur in many metal systems involves three stages of fracture: (1) crack initiation, (2) stable slow crack growth, and (3) unstable rapid crack growth. The presence of hydrogen at some critical location on the metal surface or within the metal lattice was shown to influence one or both of the first two stages of brittle fracture but has a negligible effect on the unstable rapid crack growth stage. The relative influence of the applied parameters of time, temperature, etc., on the propensity of a metal to exhibit hydrogen induced premature failure was investigated.

Nelson, H. G.↗
DOE OSTI2025

Capability in Theory, Modeling, and Validation for a Range of Innovative Fusion Concepts using High-Fidelity Moment-Kinetic Models

A computational modeling capability is created and available to the fusion community to understand and design lower-cost and innovative fusion concepts. The approach uses high- fidelity kinetic, moment-kinetic, and moment models and includes sophisticated plasma- boundary interactions. A majority of fusion-relevant simulations are performed with magnetohydrodynamic models and hybrid particle-in-cell codes, with limited-fidelity electron and kinetic physics. However, in fusion configurations like Z-pinches, field-reversed- configurations, plasma jet magneto-inertial fusion, spinning mirrors, and others, kinetic effects (both electron and ions) are critical to understand the physics and design scaling into the highly kinetic regime of a burning fusion plasma. Furthermore, as present fusion machines move towards a burning plasma regime, liquid-metal blankets are needed to handle first-wall heat- flux, reduce erosion, and eventually for energy conversion and fuel breeding. The work performed under this ARPA-E BETHE Capability Team advances the state-of-the-art in modeling and understanding plasma dynamics in fusion devices and its coupling with liquid-metal dynamics. These are critical areas of research for fusion energy to become realizable. To address these complex problems, we have leveraged and extended computational capabilities through the code, Gkeyll (developed jointly with Princeton Plasma Physics Laboratory and academic partners), for kinetic and moment modeling of fusion plasmas. The Concept Teams supported by this Capability Team include the Wisconsin High-field Axisymmetric Mirror (WHAM), Centrifugal Mirror Experiment (CFME), Plasma-Jet Magneto- Inertial Fusion (PJMIF), and solid and liquid wall plasma-material interaction studies relevant to a number of fusion concepts including Zap Energy’s Z-pinch. This software is open-source and available to the fusion community as a high-fidelity tool for the design of lower-cost fusion experiments. 3D gyrokinetic simulations of WHAM are now possible for long enough time scales to understand the evolution of interchange instabilities. 3D multi-fluid simulations of CMFE at higher Mach numbers are now possible for detailed design iterations with the goal of stability. The state-of-the-art in understanding shock formation and shock mitigation regimes in merging liners for PJMIF have been furthered by our kinetic simulations. Our novel models and frameworks studying plasma-material interaction by incorporating wall emission for various solid wall materials of relevance to pulsed and steady fusion concepts have advanced the state-of-the-art in our understanding of particle fluxes, heat fluxes, and other quantities at cathodes and anodes. The results from this work may explain discrepancies between experimental and theoretical predictions of achieved current densities in pulsed concepts such as Z-pinches. Another significant contribution of this Capability Team is the development and deployment of a novel experimental platform, LEX (Liquid Electrode eXperiment), at Virginia Tech to understand liquid metal free-surface response to electromagnetic pulses. The novel experiments along with model validation quantified the effect of different materials and sizes of liquid metal droplets on the radiative power balance of fusion plasmas for pulsed concepts. Furthermore, these experiments provided mitigation strategies for violent liquid metal response for high current pulses as would be expected in fusion regimes.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Impact of Pressure Distribution and Magnitude on the Performance of Lithium Metal Anodes

Li metal anodes are a critical battery technology due to their ability to substantially increase the energy density of Li-based batteries. It is well known that pressure greatly impacts the performance of a Li-metal anode. However, precisely how the pressure value and distribution of pressure affect performance is unclear. Furthermore, the solid-electrolyte interphase composition that forms under varying pressure distributions remains a key parameter for practical lithium metal anodes. In this work, different pressure distributions were employed by using differently shaped and oriented mechanical springs in the coin cells, resulting in varying contact points. Pressure-sensitive films were used to spatially map the pressure and correlate it to the performance. It was found that higher average pressure does not necessarily have a positive effect on performance. When high pressure is paired with poor pressure uniformity, the performance is in fact worse likely due to the current focusing effect, rendering unsatisfied cycling stability. This work points to the importance of controlling the relationship between average pressure and pressure uniformity.

25 ENERGY STORAGE↗
DOE OSTI2022

Defect and satellite characteristics of additive manufacturing metal powders

Metal additive manufacturing (AM) requires high-quality metal powders to three-dimensionally (3D) print metallic components with complex and customizable geometries. The lack of quantification of AM metal powders creates quality control challenges for 3D printed components, increases the uncertainty of printing reliability and net cost of inspected and certified printed components, and reduces the recyclability of used powders. However, critical characteristics of AM metal powders that are decisive factors for the 3D printing process, such as internal porosity, contamination, and satellite feature, remain ambiguous. In this work, we developed a novel approach to 3D quantify key characteristics of AM metal powders down to individual particles by using high-resolution synchrotron x-ray computed tomography. Empowered by the penetrative capability of high-energy x-ray, internal porosity and contamination within as-atomized metal powders from high-entropy alloys to nickel-based superalloys were evaluated. Additionally, the newly-developed dispersion method enables the homogeneous separation of individual particles, and consequently, results in the implementation of 3D particle shape analysis. To resolve a major challenge of identification and quantification of satellite-feature particles in as-atomized AM metal powders, the satellite features were quantitated by modeling and analyzing the shape parameter of local thickness variance. Furthermore, the 3D analytical methods of particle assessment in this study can be applied to other materials systems like rock, food, and pharmaceutical particles, and provide insights for process optimization across powder metallurgy, concrete, food and pharmaceutical manufacturing, and AM industries.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Self‐Strain Suppression of the Metal‐to‐Insulator Transition in Phase‐Change Oxide Devices

Strongly correlated materials exhibiting phase transitions which can be controlled through external stimuli, such as electric fields, are promising for future computing technologies beyond conventional semiconductor transistors. Devices that take advantage of structural phase transitions have inherent built‐in memory, reminiscent of synapses and neurons, and are thus natural candidates for neuromorphic computing. Of particular interest are phase‐change oxides, which allow for control over the metal‐to‐insulator transition. Here, X‐ray nano‐diffraction structural imaging of micro‐devices fabricated with the archetypal phase‐change material vanadium sesquioxide (V 2 O 3 ) is reported. The devices contain a Ga ion‐irradiated region where the metal‐to‐insulator transition critical temperature is lowered, a useful feature for controlling neuron‐like spiking behavior. Results show that strain, induced by crystal lattice mismatch between the pristine and irradiated material, leads to a suppression of the metal‐to‐insulator‐transition. Suppression occurs within the irradiated region or along its edges, depending on the defect‐distribution and the size of the region. The observed self‐straining effect can extend to other phase‐change oxides and dominate as device dimensions are reduced and become too small to dissipate strain within the irradiated region. The findings are important for phase engineering in phase‐change devices and highlight the necessity to study phase transitions at the nanoscale.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

WHA Sphere Impacting RHA Plate: Modeling Brittle Behavior in Metal Alloys

Brittle behavior of metal alloys is often critical to modeling ballistic impact and penetration. The ALEGRA multiphysics finite element software incorporates calibrated models for the equation of state, elasticity, yield stress, plasticity and fracture, but simulations do not always capture expected metal fracture. Here we report concerted efforts to do so for one important case where experiments clearly show shear fractures: a tungsten sphere impacting a steel plate at various angles. Our best simulations show fractures that are qualitatively similar to experiments, but there are significant differences in quantitative metrics. Specifically, velocities of tracers used to quantify simulated plug parameters consistently fall short of measured plug velocities. Also, simulated plugs break apart more than expected from experimental evidence. We attribute these shortfalls to the lack of an explicit shear fracture mechanism in the material models, leading to over-estimated resistance to plug formation and movement.

36 MATERIALS SCIENCE↗
DOE OSTI2020

The critical role of configurational flexibility in facilitating reversible reactive metal deposition from borohydride solutions

Development of calcium metal batteries has been historically frustrated by a lack of electrolytes capable of supporting reversible calcium electrodeposition. In this paper, we report the study of an electrolyte consisting of Ca(BH 4 ) 2 in tetrahydrofuran (THF) to gain important insight into the role of the liquid solvation environment in facilitating the reversible electrodeposition of this highly reactive, divalent metal. Through interrogation of the Ca 2+ solvation environment and comparison with Mg 2+ analogs, we show that an ability to reversibly electrodeposit metal at reasonable rates is strongly regulated by dication charge density and polarizability. Our results indicate that the greater polarizability of Ca 2+ over Mg 2+ confers greater configurational flexibility, enabling ionic cluster formation via neutral multimer intermediates. Increased concentration of the proposed electroactive species, CaBH 4 + , enables rapid and stable delivery of Ca 2+ to the electrode interface. Finally, this work helps set the stage for future progress in the development of electrolytes for calcium and other divalent metal batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Re-establishment of Sandia National Labs super-critical carbon dioxide testing autoclave capability for exposure of metal alloys and polymers (Level 4 Milestone Report)

The sCO 2 system located in 916/160A, Sandia National Laboratories, CA, was constructed in 2014, for testing of materials in the presence of supercritical carbon dioxide (sCO 2 ) at high pressures (up to 3500 psi) and temperatures (up to 650°C). The basic design of the system consists of a thermally insulated IN625 autoclave, a high-pressure supercritical CO 2 compressor, autoclave heaters, temperature controllers, gas manifold, and temperature and pressure diagnostics. This system was modified in 2016 (sCO 2 compressor was removed) to enable corrosion studies with metal alloys in gaseous CO 2 at lower pressure (up to 300 psi) at 500°C. The capability was not used much afterwards until 2020, when preliminary tests using this capability (again without the supercritical CO 2 compressor) involved the exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours in gaseous CO 2 . Using this capability, we finished experiments with low pressure (450 psi/ 3 MPa), high temperature (650°C) exposure of fatigue and tensile specimens of HN 230 and 800H alloys to CO 2 gas for 168 hours. The data from these experiments will be compared to that gathered from experiments performed in 2020 using the tube furnace and presented in a future report. It is to be noted that the tube furnace experiments ran 500-1500 hours, unlike the 168 hours of exposure in the recent experiment. This can help validate the use of the sCO 2 autoclave for both CO 2 and sCO 2 experiments.

36 MATERIALS SCIENCE↗