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DOE OSTI2025

Optimization of catholyte for halide-based all-solid-state batteries

Halide solid electrolytes gain significant attention due to their high ionic conductivity, low processing temperature, dry air compatibility, and high-voltage stability. However, low cathode active material (CAM) loading in the composite cathode constrains the realization of high energy density for halide-based all-solid-state batteries. In this study, three halide materials, raw Li 3 YBrCl 5 (LYBC-R, <30μm), milled LYBC (LYBC-M, <5 μm) and freeze-dried Li 3 InCl 6 (LIC, <500 nm), were used as catholytes, combined with LYBC-M as the electrolyte and LiIn alloy as the anode. The CAM:catholyte ratio was investigated as well as stack pressure and operating temperature. Our study demonstrates that particle size of the catholyte plays an important role only for high CAM loading or high C-rate cycling. At moderate CAM loading (65 and 70wt% LiNi 0.83 Mn 0.06 Co 0.11 O 2 ) and 0.1 C-rate, all the three catholytes perform well, providing initial discharge capacities >177 mAh/g. At high CAM loading (85wt%) and 0.1 C-rate, a cathode with the nano-scale LIC catholyte provides discharge capacity of 175 mAh/g, while the larger particle size catholytes suffer significantly reduced capacity. Both LYBC and LIC catholytes provided capacity retention >80% after 200 cycles at 0.5C. These results imply that cathode particle size is critically important for performance at high CAM loading. Furthermore, both electrolyte and cathode were tape cast to scale up size and prepare realistic layer thicknesses. A small amount of binder was used in both layers, to balance the electrochemical performance and mechanical properties. Further, the discharge capacity of a tape cell was 152mA h/g at 0.1C with a capacity retention of 81.8% after 20 cycles at 0.5C. The results demonstrate the excellent performance of LYBC as an electrolyte, and provide guidance for halide-based cathode design.

25 ENERGY STORAGE↗

DOE OSTI2024

Microstructural refinement of an Al-Ce-Mg alloy via Shear Assisted Processing and Extrusion

Al-Ce alloys have attracted recent interest because of their high thermal stability due to the low solubility of Ce in the Al matrix. The Al 11 Ce 3 eutectic phase gives excellent strain hardening behavior and moderate high-temperature strength in the as-cast state. However, its strengthening effect is limited by its coarse as-cast structure. Therefore, alternative manufacturing methods such as additive manufacturing or equal channel angular pressing have been applied to refine the Al 11 Ce 3 phase to good effect. However, these techniques are both expensive and time-consuming. Therefore, this study aims to use Shear Assisted Processing and Extrusion (ShAPE), an emerging solid phase processing technique that is more easily scalable than the previously mentioned methods. ShAPE can produce useful cross-sections of an Al-8Ce-4Mg alloy while refining the Al 11 Ce 3 phase to produce a higher strength material. It was found that a low temperature ShAPE process can improve the room temperature yield strength by ~60 % compared to a binary Al-4Mg alloy. Additionally, the high-temperature yield strength of the Al-Ce alloys increased by 20%, with a simultaneous 15% improvement in ductility compared to the binary Al-Mg alloy. Finally, these results highlight the potential for ShAPE as a processing technique for Al-Ce alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Wrought Aluminum-Cerium Alloys by Shear Assisted Processing and Extrusion

Al-Ce alloys have attracted recent interest because of their high thermal stability due to the very low solubility of Ce in the Al matrix. The Al 11 Ce 3 eutectic phase gives excellent strain hardening behavior and moderate high-temperature strength in the as-cast state. However, its strengthening effect is limited by its coarse as-cast structure. Therefore, alternative manufacturing methods such as additive manufacturing or equal channel angular pressing have been applied to refine the Al 11 Ce 3 phase to good effect. However, these techniques are both expensive and time-consuming. Therefore, this study aims to use Shear Assisted Processing and Extrusion (ShAPE), an emerging solid phase processing technique that is more easily scalable than the previously mentioned methods. ShAPE can produce useful cross-sections of an Al-8Ce-4Mg alloy while refining the Al 11 Ce 3 phase to produce a higher strength material. It was found that a low temperature ShAPE process can improve the room temperature yield strength by ~60% compared to a binary Al-4Mg alloy. Additionally, the high-temperature yield strength of the Al-Ce alloys increased by 20%, with a simultaneous 15% improvement in ductility compared to the binary Al-Mg alloy. These results highlight the potential for ShAPE as a processing technique for Al-Ce alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Spatially-resolved lithiation dynamics from operando X-ray diffraction and electrochemical modeling of lithium-ion cells

In this study, energy dispersive X-ray diffraction is used to profile the time evolution of ordered Li x C 6 phases in solid electrodes of lithium-ion cells charged at rates between 0.2 and 4.7C (where 1C corresponds to full discharge in 1 h). The methods for quantifying lithium concentration in these phases from the acquired diffraction patterns are described. Compact expressions for time-dependent concentration gradients in the solid electrodes using orthogonal polynomial expansions are presented. Experimentally, these gradients persisted in lithiated graphite electrodes even after the cells rested at open-circuit for over 9 h. A multiphase electrochemical model of graphite intercalation captured many of the observed behaviors, including the progression of phase transitions and the persistent gradients at zero current. However, the magnitude of concentration gradients in both the oxide cathode and graphite anode is underestimated by the model, even at moderate currents.

25 ENERGY STORAGE↗

DOE OSTI2026

Understanding the effect of friction stir processing on electrical steel: Microstructural changes and mechanical transformations

Raising Si beyond 3.5 wt% reduces core loss but embrittles electrical steels, constraining processing and application. Here we assess friction stir processing (FSP) as a solid‑state route to enable Fe–4.0 wt% Si with improved mechanical performance. Temperature‑controlled FSP with a PcBN tool produced a defect‑free processed zone. SEM/EBSD revealed dynamic recrystallization and grain refinement from an average 110 μm in the base material to ∼20 μm in the processed region, with ∼ 80% of grains < 40 μm and a reduction in high‑angle boundary fraction to ∼65% (vs >85% in the base). Comparative mechanical property analysis shows a moderate increase in yield strength in FSP samples relative to the base material, with a significant improvement in ductility (∼35–50%). Post‑fracture EBSD identified 60° twin boundaries in the base while sub-grain formation with elevated KAM in the FSP sample. Fractography revealed a shift from quasi‑cleavage in the Base-faceted planes with river patterns, steps, and occasional secondary cracks—to ductile micro void coalescence after FSP. Following FSP, the material retains soft‑magnetic behavior, with modest shifts in saturation magnetization consistent with grain refinement and stored strain, accompanied by a clear gain in formability. These results indicate that FSP provides a viable route to deploy higher‑Si electrical steels with concurrent gains in strength and ductility.

Electrical steel↗

NASA NTRS1994

Plasma produced by impacts of fast dust particles on a thin film

The thin-film impact plasma detector was pioneered by Berg for detecting small cosmic dust particles and measuring their approximate velocities in a time-of-flight configuration. While Berg's device was highly successful in establishing the flux of interplanetary dust, the accuracy of measuring the velocities of individual particles was a moderate 18 percent in magnitude and 27 degrees in angle. A much greater accuracy of less than or equal to 1 percent in determining the velocity components appears desirable in order to associate a particle with its parent body. In order to meet that need, research was initiated to determine if a thin-film detector can be designed to provide such accurate velocity measurements. Previous laboratory investigations of the impact plasma uncovered two difficulties: (1) solid or liquid spray is ejected from a primary impact crater and strikes neighboring walls where it produces secondary impact craters and plasma clouds; as a result, both quantity and time of detection of the plasma can vary significantly with the experiment configuration. Particles from an accelerator rarely have speeds v greater than or equal to 10-15 km/s, while cosmic dust particles typically impact at v = 10-72 km/s. The purpose of the tests discussed in this paper was to resolve the two difficulties mentioned. That is, the experiment configuration was designed to reduce the contribution of plasma from secondary impacts. In addition, most particles with v less than or equal to 25 km/s and all particles with v less than or equal to 10 km/s were eliminated from the beam.

Auer, Siegfried↗

DOE OSTI2026

Cs X Si 15 P 21 ( X = Sn or Pb): Polar Noncentrosymmetric Si–P Frameworks Stabilized by Covalent X –P Bonding

Metal silicon phosphides composed of earth-abundant Si and P tend to exhibit semiconducting properties and adopt diverse crystal structures with relatively small additions of structure-directing elements. The potential of silicon phosphide materials in nonlinear optical applications has been hindered by the inability to systematically produce noncentrosymmetric structures with such a flexible framework. Here, in this work, two isostructural compounds with a novel noncentrosymmetric structure were made possible by the inclusion of elements with stereochemically active lone pairs (Sn 2+ and Pb 2+ ). The structures were determined through single-crystal and synchrotron powder X-ray diffraction. Analysis of chemical bonding in real space through the electron localization function revealed stereochemically active Pb 2+ and Sn 2+ species in a trigonal pyramidal coordination with {Pb/Sn}–P bonds. Such covalent bonding between Pb and P is quite uncommon in extended solids and has been reported in a few rare instances. Band structure calculations and linear optical measurements confirm the semiconducting nature of Cs X Si 15 P 21 ( X = Sn or Pb). The synthesis was optimized to yield high-purity polycrystalline samples. The nonlinear optical properties show promising second-harmonic generation (SHG) coefficients from the Kurtz–Perry method. First-principles calculations of the nonlinear optical properties support the experimentally determined SHG values and provide moderate values of birefringence, suggesting Cs X Si 15 P 21 could be phase-matchable and practical nonlinear optical materials in the mid-IR region.

crystal structure↗

DOE OSTI2022

Influence of nuclear quantum effects on the electronic properties of amorphous carbon

We carry out quantum simulations to study the physical properties of diamond-like amorphous carbon by coupling first-principles molecular dynamics with a quantum thermostat, and we analyze multiple samples representative of different defective sites present in the disordered network. We show that quantum vibronic coupling is critical in determining the electronic properties of the system, in particular its electronic and mobility gaps, while it has a moderate influence on the structural properties. We find that despite localized electronic states near the Fermi level, the quantum nature of the nuclear motion leads to a renormalization of the electronic gap surprisingly similar to that found in crystalline diamond. We also discuss the notable influence of nuclear quantum effects on band-like and variable-hopping mechanisms contributing to electrical conduction. Our calculations indicate that methods often used to evaluate electron–phonon coupling in ordered solids are inaccurate to study the electronic and transport properties of amorphous semiconductors composed of light atoms.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

NASA NTRS2004

New Nickel Vapor Pressure Measurements: Possible Implications for Nebular Condensates

Temperatures high enough to vaporize even refractory solids existed in the midplane of the solar nebula during its earliest evolutionary stages and played an important role in the processing of materials that went into the formation of the inner planets and asteroids. A variety of such high-T materials have been identified in primitive chondritic meteorites. These include chemically zoned FeNi metal grains that are generally believed to have formed directly by gas-solid condensation from a gas of approximately solar composition. These FeNi particles provide important information about the times scales of formation and physical transport mechanisms in the nebula, as well as formation temperature, pressure and gas chemistry. Currently, however, the interpretation of the chemical signatures in these FeNi particles rests on less than perfect information about the condensation sequence of siderophile elements. For example much, if not all, of the thermodynamic data for the vapor pressures of moderately refractory metals , such as Fe, Ni and Co, do not cover the desired temperature range. As a result, quite large extrapolations are needed. These extrapolations can be complex and uncertain due to factors such as oxygen fugacity or the presence of hydrogen gas.

Johnson, N. M.↗

NASA NTRS2007

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.↗

DOE OSTI2023

Solid‐Adsorbed Polymer‐Electrolyte Interphases for Stabilizing Metal Anodes in Aqueous Zn and Non‐Aqueous Li Batteries

Abstract Polymers are known to adsorb spontaneously from liquid solutions in contact with high‐energy substrates to form configurationally complex, but robust phases that often exhibit higher durability than might be expected from the individual physical bonds formed with the substrate. Rational control of the physical, chemical, and transport properties of such interphases has emerged as a fundamental opportunity for scientific and technological advances in energy storage technology but requires in‐depth understanding of the conformation states and electrochemical effect of the adsorbed polymers. Here, we analyze the interfacial adsorption of oligomeric polyethylene glycol (PEG) chains of moderate sizes dissolved in protic and aprotic liquid electrolytes and find that there is an optimum polymer molecular weight of approximately 400 Da at which the highest columbic efficiency is achieved for both Zn and Li deposition. These findings point to a simple, versatile approach for extending the lifetime of batteries.

Jin, Shuo↗

DOE OSTI2020

Characteristics of flow through randomly packed impermeable and permeable particles using pore resolved simulations

Pore resolved simulations are performed to study the mean flow characteristics in porous media formed by random distribution of impermeable and permeable particles. Here, permeability of the medium and reactive surface areas are analyzed for a range of solid fractions, packing patterns and flow rates. The results are compared with models presented in the literature and with simulations of flow through ordered packings. Permeability of a randomly packed porous medium is found to depend on the heterogeneous distribution of porosity which results from particle agglomeration and is typically ignored by simpler models. The reactive surface area is dependent on the flow field at pore scale in addition to geometry. Moreover, the wake formed downstream of the particles at moderately high flow rates also affects the reactive surface area. Similar analysis is also performed by assuming particles to be permeable to account for dual scale porosity relevant for various engineering applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1991

Oxygen extraction from lunar soil by fluorination

Mining and processing of lunar material could possibly lead to more cost-efficient scenarios for permanent presence of man in space and on the Moon. Production of oxygen for use as propellant seems especially important. Different candidate processes for oxygen-extraction from lunar soil were proposed, of which the reduction of ilmenite by hydrogen was studied most. This process, however, needs the concentration of ilmenite from lunar regolith to a large extent and releases oxygen only with low efficiency. Another possibility - the fluorination method - which works with lunar bulk material as feedstock is discussed. Liberation of oxygen from silicate or oxide materials by fluorination methods has been applied in geoscience since the early sixties. The fact that even at moderate temperatures 98 to 100 percent yields can be attained, suggests that fluorination of lunar regolith could be an effective way of propellant production. Lunar soil contains about 50 percent oxygen by weight which is gained nearly completely through this process as O2 gas. The second-most element Si is liberated as gaseous SiF4. It could be used for production of Si-metal and fluorine-recycling. All other main elements of lunar soil will be converted into solid fluorides which also can be used for metal-production and fluorine-recycling. Preliminary results of small scale experiments with different materials are discussed, giving information on specific oxygen-yields and amounts of by-products as functions of temperature. These experiments were performed with an already existing fluorine extraction and collection device at the University of Bonn, normally used for determination of oxygen-isotopic abundances. Optimum conditions, especially concerning energy consumption, are investigated. Extrapolation of the experimental results to large industrial-type plants on the Moon is tried and seems to be promising at first sight. The recycling of the fluorine is, however, crucial for the process. It might be achieved by means of electrolysis. This needs further investigation. The technical problem of transport and handling of the toxic and corrosive fluorine seems to be solvable and could be done by inert storage vessels.

Seboldt, W.↗

NASA NTRS2011

Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

Orzechowska, G. E.↗

NASA NTRS2020

Monitoring Water-Related Ecosystems with Earth Observation Data in Support of Sustainable Development Goal (SDG) 6 Reporting

Lack of national data on water-related ecosystems is a major challenge to achieving the Sustainable Development Goal (SDG) 6 targets by 2030. Monitoring surface water extent, wetlands, and water quality from space can be an important asset for many countries in support of SDG 6 reporting. We demonstrate the potential for Earth observation (EO) data to support country reporting for SDG Indicator 6.6.1, ‘Change in the extent of water-related ecosystems over time’ and identify important considerations for countries using these data for SDG reporting. The spatial extent of water-related ecosystems, and the partial quality of water within these ecosystems is investigated for seven countries. Data from the Moderate Resolution Imaging Spectroradiometer (MODIS) and Landsat 5, 7, and 8 with Shuttle Radar Topography Mission (SRTM) are used to measure surface water extent at 250 m and 30 m spatial resolution, respectively, in Cambodia, Jamaica, Peru, the Philippines, Senegal, Uganda, and Zambia. The extent of mangroves is mapped at 30 m spatial resolution using Landsat 8 Operational Land Imager (OLI), Sentinel-1, and SRTM data for Jamaica, Peru, and Senegal. Using Landsat 8 and Sentinel 2A imagery, total suspended solids and chlorophyll-a are mapped over time for a select number of large surface water bodies in Peru, Senegal, and Zambia. All of the EO datasets used are of global coverage and publicly available at no cost. The temporal consistency and long time-series of many of the datasets enable replicability over time, making reporting of change from baseline values consistent and systematic. We find that statistical comparisons between different surface water data products can help provide some degree of confidence for countries during their validation process and highlight the need for accuracy assessments when using EO-based land change data for SDG reporting. We also raise concern that EO data in the context of SDG Indicator 6.6.1 reporting may be more challenging for some countries, such as small island nations, than others to use in assessing the extent of water-related ecosystems due to scale limitations and climate variability. Country-driven validation of the EO data products remains a priority to ensure successful data integration in support of SDG Indicator 6.6.1 reporting. Multi-country studies such as this one can be valuable tools for helping to guide the evolution of SDG monitoring methodologies and provide a useful resource for countries reporting on water-related ecosystems. The EO data analyses and statistical methods used in this study can be easily replicated for country-driven validation of EO data products in the future.

water-related ecosystems; surface water extent; ma↗

NASA NTRS2020

Monitoring Water-Related Ecosystems with Earth Observation Data in Support of Sustainable Development Goal (SDG) 6 Reporting

Lack of national data on water-related ecosystems is a major challenge to achieving the Sustainable Development Goal (SDG) 6 targets by 2030. Monitoring surface water extent, wetlands, and water quality from space can be an important asset for many countries in support of SDG 6reporting. We demonstrate the potential for Earth observation (EO) data to support country reporting for SDG Indicator 6.6.1, ‘Change in the extent of water-related ecosystems over time’ and identify important considerations for countries using these data for SDG reporting. The spatial extent of water-related ecosystems, and the partial quality of water within these ecosystems is investigated for seven countries. Data from the Moderate Resolution Imaging Spectroradiometer (MODIS) and Landsat 5, 7, and 8 with Shuttle Radar Topography Mission (SRTM) are used to measure surface water extent at 250 m and 30 m spatial resolution, respectively, in Cambodia, Jamaica, Peru, the Philippines, Senegal, Uganda, and Zambia. The extent of mangroves is mapped at 30 m spatial resolution using Landsat 8 Operational Land Imager (OLI), Sentinel-1, and SRTM data for Jamaica, Peru, and Senegal. Using Landsat 8 and Sentinel 2A imagery, total suspended solids and chlorophyll-a are mapped overtime for a select number of large surface water bodies in Peru, Senegal, and Zambia. All of the EO datasets used are of global coverage and publicly available at no cost. The temporal consistency and long time-series of many of the datasets enable replicability over time, making reporting of change from baseline values consistent and systematic. We find that statistical comparisons between different surface water data products can help provide some degree of confidence for countries during their validation process and highlight the need for accuracy assessments when using EO-based land change data for SDG reporting. We also raise concern that EO data in the context of SDG Indicator 6.6.1reporting may be more challenging for some countries, such as small island nations, than others to use in assessing the extent of water-related ecosystems due to scale limitations and climate variability. Country-driven validation of the EO data products remains a priority to ensure successful data integration in support of SDG Indicator 6.6.1 reporting. Multi-country studies such as this one can be valuable tools for helping to guide the evolution of SDG monitoring methodologies and provide a useful resource for countries reporting on water-related ecosystems. The EO data analyses and statistical methods used in this study can be easily replicated for country-driven validation of EO data products in the future.

Raha Hakimdavar↗

DOE OSTI2023

Solid–Adsorbed Polymer–Electrolyte Interphases for Stabilizing Metal Anodes in Aqueous Zn and Non–Aqueous Li Batteries

Polymers are known to adsorb spontaneously from liquid solutions in contact with high-energy substrates to form configurationally complex, but robust phases that often exhibit higher durability than might be expected from the individual physical bonds formed with the substrate. Rational control of the physical, chemical, and transport properties of such interphases has emerged as a fundamental opportunity for scientific and technological advances in energy storage technology but requires in-depth understanding of the conformation states and electrochemical effect of the adsorbed polymers. Here, we analyze the interfacial adsorption of oligomeric polyethylene glycol (PEG) chains of moderate sizes dissolved in protic and aprotic liquid electrolytes and find that there is an optimum polymer molecular weight of approximately 400 Da at which the highest columbic efficiency is achieved for both Zn and Li deposition. Furthermore, these findings point to a simple, versatile approach for extending the lifetime of batteries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1992

Hybrid rocket performance

A hybrid rocket is a system consisting of a solid fuel grain and a gaseous or liquid oxidizer. Figure 1 shows three popular hybrid propulsion cycles that are under current consideration. NASA MSFC has teamed with industry to test two hybrid propulsion systems that will allow scaling to motors of potential interest for Titan and Atlas systems, as well as encompassing the range of interest for SEI lunar ascent stages and National Launch System Cargo Transfer Vehicle (NLS CTV) and NLS deorbit systems. Hybrid systems also offer advantages as moderate-cost, environmentally acceptable propulsion system. The objective of this work was to recommend a performance prediction methodology for hybrid rocket motors. The scope included completion of: a literature review, a general methodology, and a simplified performance model.

Frederick, Robert A., Jr.↗