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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 415 records · Page 23

Solid-State Recrystallization Pathways of Sodium Aluminate Hydroxy Hydrates

Crystallization of Al-bearing solid phases from highly alkaline Na 2 O:Al 2 O 3 :H 2 O solutions commonly necessitates an Al 3+ coordination change from tetrahedral to octahedral, but intermediate coordination states are often difficult to isolate. Here, a similar Al 3+ coordination change process is examined during the solid-state recrystallization of sodium oxohydroxoaluminate hydrate (MSA) to nonasodium bis(hexahydroxy aluminate) trihydroxide hexahydrate (NSA) at ambient temperature. While the MSA structure contains solely polymerized tetrahedral Al 3+ , the NSA structure is a molecular aluminate salt solely based upon monomeric octahedral Al 3+ . Spontaneous recrystallization of MSA and excess sodium hydroxide hydrate into NSA over 3 days of reaction time was clearly evident in X-ray diffractograms and in Raman spectra. In situ 27 Al multiple quantum MAS NMR spectroscopy showed no evidence of intermediate aluminates, suggesting that intermediates, such as pentacoordinate Al 3+ , are short-lived and require more highly time resolved spectroscopies to detect. Such research is advancing upon detailed mechanistic understanding of Al 3+ coordination change mechanisms in these highly alkaline systems, with relevance to aluminum refining, corrosion sciences, and nuclear waste processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Initial Study of Friction Pull Plug Welding

Pull plug friction welding is a new process being developed to conveniently eliminate defects from welded plate tank structures. The general idea is to drill a hole of precise, optimized dimensions and weld a plug into it, filling the hole perfectly. A conically-shaped plug is rotated at high angular velocity as it is brought into contact with the plate material in the hole. As the plug is pulled into the hole, friction rapidly raises the temperature to the point at which the plate material flows plastically. After a brief heating phase, the plug rotation is terminated. The plug is then pulled upon with a forging force, solidly welding the plug into the hole in the plate. Three aspects of this process were addressed in this study. The transient temperature distribution was analyzed based on slightly idealized boundary conditions for different plug geometries. Variations in hole geometry and ram speed were considered, and a program was created to calculate volumes of displaced material and empty space, as well as many other relevant dimensions. The relation between the axially applied forging force and the actual forging pressure between the plate and plug surfaces was determined for various configurations.

Rich, Brian S.↗

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy↗

Integrated Multiscale Model for Design of Robust 3D Solid-state Lithium Batteries

In FY23, we successfully established the multiscale modeling framework for probing the effects of materials microstructure on cell performance of 3D solid-state batteries. The framework covers physicochemical processes co-evolving at the atomistic and microstructure scales. Our simulations revealed the mechanism of initial interfacial degradation, formation of secondary phases, and the structure-property relationship for ion transport and mechanical stability at the interface. In addition, we also established the microstructure-performance relationships by performing sensitivity tests of various microstructure features and extracting their impact on cell performance during charge-discharge cycles. We have successfully applied our multiscale, multiphysics modeling capability to common electrode and electrolyte materials that are of interests to VTO and the experimental teams within the US-Germany collaboration. The insights we obtained from these simulations provide valuable design principles to optimize materials properties for advanced 3D solid-state batteries.

25 ENERGY STORAGE↗

CO 2 Laser Sintering of Garnet-Type Solid-State Electrolytes

We report the processing of garnet-type solid-state electrolytes remains challenging as densification conventionally requires high sintering temperatures and long processing times, which can result in severe Li loss, the formation of secondary phases, and thus high porosity and low ionic conductivity. Here, we report an ultrafast sintering method based on CO 2 laser scanning with the assistance of a heating stage. We demonstrate the rapid densification of low-packing-density Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) films, which are difficult to densify by conventional furnace sintering methods. This unique approach has three fingerprint characteristics: (1) mitigation of Li loss through ultrafast sintering (dwelling time $\ll$1 s); (2) a unique anisotropic shrinkage behavior that greatly reduces film thickness; (3) wave-like surface topology from point scanning strategy that enables 3D interfacial contacts with electrode materials. Herein, highly dense (95.68%) and highly conductive (0.26 mS·cm –1 at 25 °C) LLZTO films are obtained through CO2 laser sintering. This work provides a unique, scalable, and widely applicable ultrarapid laser sintering technique to overcome the difficulties associated with classic methods for the integration of SSEs for practical all-solid-state Li-metal battery applications.

36 MATERIALS SCIENCE↗

Analysis of minerals containing dissolved traces of the fluid phase components water and carbon dioxide

Substantial progress has been made towards a better understanding of the dissolution of common gas/fluid phase components, notably H2O and CO2, in minerals. It has been shown that the dissolution mechanisms are significantly more complex than currently believed. By judiciously combining various solid state analytical techniques, convincing evidence was obtained that traces of dissolved gas/fluid phase components undergo, at least in part, a redox conversion by which they split into reduced H2 and and reduced C on one hand and oxidized oxygen, O(-), on the other. Analysis for 2 and C as well as for any organic molecules which may form during the process of co-segregation are still impeded by the omnipresent danger of extraneous contamination. However, the presence of O(-), an unusual oxidized form of oxygen, has been proven beyond a reasonable doubt. The presence of O(-) testifies to the fact that a redox reaction must have taken place in the solid state involving the dissolved traces of gas/fluid phase components. Detailed information on the techniques used and the results obtained are given.

Freund, Friedemann↗

Ultrafast Sintering and Dopant Effects in Garnet LLZO Solid Electrolytes

High-throughput, low-cost manufacturing, and optimization of solid electrolytes are necessary for the adoption of solid-state batteries. In this work, garnet-type Li 7 La 3 Zr 2 O 12 (LLZO) with different aliovalent dopants, 𝑇𝑎$_{^·_{𝑍𝑟}}$, 𝐴𝑙$^{··}_{𝐿𝑖}$, and 𝐺𝑎$^{··}_{𝐿𝑖}$, have been ultrafast-sintered with different temperature ramping rates. The densification behavior, phases, their evolution, and surface chemistry of different LLZO have been investigated and linked to their electrochemical performances. It has been shown that LLZO with 𝑇𝑎$_{^·_{𝑍𝑟}}$ dopant demonstrates the highest garnet phase purity and overall best electrochemical performances, and ultrafast sintering further improves densification, ionic conductivity, and electrochemical stability. On the other hand, LLZO doped with 𝐴𝑙$^{··}_{𝐿𝑖}$ and 𝐺𝑎$^{··}_{𝐿𝑖}$ are reaching higher cubic phase purities and ionic conductivities via conventional sintering, indicating undesirable dopant migration and segregation during the ultrafast sintering process. In conclusion, these findings provide insights into the manufacturing of solid electrolyte materials.

36 MATERIALS SCIENCE↗

Advances and perspectives on mass transfer and enzymatic hydrolysis in the enzyme-mediated lignocellulosic biorefinery: A review

We report enzymatic hydrolysis is a critical process for the cellulase-mediated lignocellulosic biorefinery to produce sugar syrups that can be converted into a whole range of biofuels and biochemicals. Such a process operating at high-solid loadings (i.e., scarcely any free water or roughly ≥ 15% solids, w/w) is considered more economically feasible, as it can generate a high sugar concentration at low operation and capital costs. However, this approach remains restricted and incurs “high-solid effects”, ultimately causing the lower hydrolysis yields with increasing solid loadings. The lack of available water leads to a highly viscous system with impaired mixing that exhibits strong transfer resistance and reaction limitation imposed on enzyme action. Evidently, high-solid enzymatic hydrolysis involves multi-scale mass transfer and multi-phase enzyme reaction, and thus requires a synergistic perspective of transfer and biotransformation to assess the interactions among water, biomass components, and cellulase enzymes. Porous particle characteristics of biomass and its interface properties determine the water form and distribution state surrounding the particles, which are summarized in this review aiming to identify the water-driven multi-scale/multi-phase bioprocesses. Further aided by the cognition of rheological behavior of biomass slurry, solute transfer theories, and enzyme kinetics, the coupling effects of flow-transfer-reaction are revealed under high-solid conditions. Based on the above basic features, this review lucidly explains the causes of high-solid hydrolysis hindrances, highlights the mismatched issues between transfer and reaction, and more importantly, presents the advanced strategies for transfer and reaction enhancements from the viewpoint of process optimization, reactor design, as well as enzyme/auxiliary additive customization.

45 multi-scale, multi-phase, enzymatic reaction↗

Solid-state transformations during laser directed energy deposition of Ti-6Al-4V powder hydride-dehydrided from scrap metals

During laser directed energy deposition (DED-LB), thermal cycling and powder chemical composition produce distinct thermal histories, which vary mechanical properties. Using real-time X-ray diffraction, this study investigates solid-state transformations during DED-LB to understand process-structure-property relationships for angular Ti-6Al-4V powder hydride–dehydrided from scrap metals. Results showed that regions near the molten pool experienced high cooling rates, leading to martensitic transformation from the β phase and increased hardness. Regions farther from the molten pool underwent tempering without solid-state transformation and decreased hardness. These findings support alternative feedstocks for metal additive manufacturing for a circular economy and resilient supply chains.

Additive manufacturing (AM)↗

The TLK-ASF1 histone chaperone pathway plays a critical role in IL-1β–mediated AML progression

Identifying and targeting microenvironment-driven pathways that are active across acute myeloid leukemia (AML) genetic subtypes should allow the development of more broadly effective therapies. The proinflammatory cytokine interleukin-1β (IL-1β) is abundant in the AML microenvironment and promotes leukemic growth. Through RNA-sequencing analysis, we identify that IL-1β–upregulated ASF1B (antisilencing function-1B), a histone chaperone, in AML progenitors compared with healthy progenitors. ASF1B, along with its paralogous protein ASF1A, recruits H3-H4 histones onto the replication fork during S-phase, a process regulated by Tousled-like kinase 1 and 2 (TLKs). Although ASF1s and TLKs are known to be overexpressed in multiple solid tumors and associated with poor prognosis, their functional roles in hematopoiesis and inflammation-driven leukemia remain unexplored. In this study, we identify that ASF1s and TLKs are overexpressed in multiple genetic subtypes of AML. We demonstrate that depletion of ASF1s significantly reduces leukemic cell growth in both in vitro and in vivo models using human cells. Using a murine model, we show that overexpression of ASF1B accelerates leukemia progression. Moreover, Asf1b or Tlk2 deletion delayed leukemia progression, whereas these proteins are dispensable for normal hematopoiesis. Through proteomics and phosphoproteomics analyses, we uncover that the TLK-ASF1 pathway promotes leukemogenesis by affecting the cell cycle and DNA damage pathways. Collectively, our findings identify the TLK1-ASF1 pathway as a novel mediator of inflammatory signaling and a promising therapeutic target for AML treatment across diverse genetic subtypes. Finally, selective inhibition of this pathway offers potential opportunities to intervene effectively, address intratumoral heterogeneity, and ultimately improve clinical outcomes in AML.

60 APPLIED LIFE SCIENCES↗

The source and origin of the exotic component and KREEP-rich materials on the moon

The enrichments of trace-element concentrations in lunar soils are attributed to the combined effects of comminution of local rocks and a preferential addition of the exotic component to finer grain sizes. The exotic component appears similar to Fra Mauro materials, and there is a strong correlation between the percentage of exotic component and distance from the Fra Mauro site. Based on trace-element characteristics, it is suggested that the exotic component is finely comminuted KREEP and is dispersed on the lunar surface from the Fra Mauro and other high gamma-ray active regions in the Imbrium-Procellarum regions. The major and trace-element chemistry of these materials is considered to be due to impact melting of trace-element-rich accessory phases followed by variable dilution with partial melts of the bulk solid phases of plagioclase, low-Ca pyroxene, and olivine. The generation of KREEP and the exotic component is an impact-produced local process and need not imply a global occurrence of radioactive crust on the moon.

Murthy, V. R.↗

Precision aqueous cleaner for RSRM

Chlorinated solvents such as freon and 1,1,1 trichloroethane (TCA) are both environmental and physiological hazards which deplete stratospheric ozone. These chemicals are the primary degreasing solvents (vapor, vat, and hand operations) in redesigned solid rocket motor (RSRM) manufacturing. Due to the mandates of the Clean Air Act, substitutes must be identified for RSRM cleaning processes. The initial phase of laboratory testing identified candidate cleaners to replace 1,1,1 trichloroethane for cleaning, potentially reducing annual TCA consumption by 800,000 lbs. This paper describes RSRM testing which elucidated the effects of several interdependent variable including: definition of surface cleanliness criteria, validation of cleaning power of new candidates, the effect of immersion cleaning versus spray cleaning on cleaning, any effect of the cleaner and/or inhibitor upon bondline aging, and compatibility of the cleaners with nonmetallic tooling and processing materials.

Hutchens, D. E.↗

Tribological Performance of PM300 Solid Lubricant Bushings for High Temperature Applications

PM300 is a high temperature solid lubricant material produced through conventional powder metallurgy processing. PM300 is a combination of metal binder (NiCr), hardener (Cr2O3) and lubricant (Ag and BaF2/CaF2) phases and is in commercial use in high temperature furnace conveyors. In this paper, the tribological characteristics of PM300 are evaluated using a newly developed bushing test rig in which PM300 bushings are loaded against rotating steel shafts at temperatures from 25 to 650 C. The data shows that friction and wear are low to moderate and that the lubrication performance (friction) improves with increasing temperature. Several alternative PM300 compositions are evaluated which do not contain silver and are targeted at aircraft gas turbine applications in which environmental compatibility of silver is a concern. It is expected that the data resulting from this research will further the commercialization of this technology.

Striebing, Donald R.↗

An integrated optical CO2 sensor. Phase 0: Design and fabrication of critical elements

Significant progress has been made toward all of the goals for the first phase of the project short of actual fabrication of a light path. Two alternative approaches to fabricating gold mirrors using the basic LIGA process were developed, one using electroplated solid gold mirrors and the second using gold plated over a nickel base. A new method of fabrication, the transfer mask process, was developed and demonstrated. Analysis of the projected surface roughness and beam divergence effects was completed. With gold surface with low surface roughness scattering losses are expected to be insignificant. Beam divergence due to diffraction will require a modification of the original design, but should be eliminated by fabricating mirrors 1000 mu m in height by 1000 mu m in width and using a source with an initial beam radius greater than 300 mu m. This may eliminate any need for focusing optics. Since the modified design does not affect the mask layout, ordering of the mask and fabrication of the test structures can begin immediately at the start of Phase 1.

Murphy, Michael C.↗

Anomalous thermoelectricity at the two-dimensional structural transition of SnSe monolayers

The thermoelectric figure of merit ZT comprises electronic and vibrational contributions that drastically change across phase transitions, and the most common theoretical ab initio approach to thermoelectricity fails to describe the evolution of ZT across finite-temperature structural transitions in its entirety. Furthermore, while the thermoelectric behavior of bulk SnSe has been extensively studied, SnSe monolayers have been experimentally realized only recently, and the existent prediction of thermoelectricity on this two-dimensional material is unreliable because it misses its structural transition altogether. SnSe monolayers (and similar GeS, GeSe, GeTe, SnS, and SnTe monolayers) experience a temperature-induced two-dimensional Pnm2 1 → P4/nmm structural transition precipitated by the softening of vibrational modes, and we describe their thermoelectric properties across the phase transition, using molecular dynamics data to inform both electronic and vibrational coefficients directly and within the same footing. Similar to recent experimental observations pointing to an overestimated ZT past the transition temperature in bulk SnSe, we find a smaller ZT on SnSe monolayers when compared to its value predicted by the standard paradigm, due to the dramatic changes in the electrical conductivity and lattice thermal conductivity as the structural transition ensues. Here, the process described here lends a strong focus to both the vibrational and electronic evolutions throughout the structural transition, and it applies to thermoelectric materials undergoing thermally driven solid-to-solid structural phase transitions in one, two, and three dimensions.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Separation of Radionuclides from a Rare Earth-Containing Solution by Zeolite Adsorption

The increasing industrial demand for rare earths requires new or alternative sources to be found. Within this context, there have been studies validating the technical feasibility of coal and coal byproducts as alternative sources for rare earth elements. Nonetheless, radioactive materials, such as thorium and uranium, are frequently seen in the rare earths’ mineralization, and causes environmental and health concerns. Consequently, there exists an urgent need to remove these radionuclides in order to produce high purity rare earths to diversify the supply chain, as well as maintain an environmentally-favorable extraction process for the surroundings. In this study, an experimental design was generated to examine the effect of zeolite particle size, feed solution pH, zeolite amount, and contact time of solid and aqueous phases on the removal of thorium and uranium from the solution. The best separation performance was achieved using 2.50 g of 12-µm zeolite sample at a pH value of 3 with a contact time of 2 h. Under these conditions, the adsorption recovery of rare earths, thorium, and uranium into the solid phase was found to be 20.43 wt%, 99.20 wt%, and 89.60 wt%, respectively. The Freundlich adsorption isotherm was determined to be the best-fit model, and the adsorption mechanism of rare earths and thorium was identified as multilayer physisorption. Further, the separation efficiency was assessed using the response surface methodology based on the development of a statistically significant model.

58 GEOSCIENCES↗

Scientific support for an orbiter middeck experiment on solid surface combustion

The objective is to determine the mechanism of gas-phase flame spread over solid fuel surfaces in the absence of any buoyancy or externally imposed gas-phase flow. Such understanding can be used to improve the fire safety aspects of space travel by providing information that will allow judicious selections of spacecraft materials and environments to be made. The planned experiment consists of measuring the flame spread rate over thermally thin and thermally thick fuels in a closed container in the low-gravity environment of the Space Shuttle. Measurements consist of flame spread rate and shape obtained from two views of the process as recorded on movie film and surface and gas-phase temperatures obtained from fine-wire thermocouples. The temperature measurements along with appropriate modeling provide information about the gas-to-solid heat flux. Environmental parameters to be varied are the oxygen concentration and pressure.

Altenkirch, Robert A.↗