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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

Characterizing Martian X-Ray Amorphous Materials Through Terrestrial Analogs

X-ray amorphous materials (i.e., lacking long-range crystallographic order) have been identified on the martian surface from orbit and in-situ. Initial models of orbital IR spectral data identified volcanic glasses [e.g., 1], but subsequent interpretations suggested that amorphous silicates are dominantly secondary in nature and formed from water-rock interactions [e.g., 2-4]. Thermal IR spectra from the Mini-Thermal Emission Spectrometer on the Spirit rover show evidence for the amorphous secondary product opaline silica [e.g., 5]. X-ray diffraction (XRD) measurements by the CheMin instrument on the Mars Science Laboratory rover have identified 20-70 wt.% amorphous materials in every sample analyzed in Gale crater to date [e.g., 6]. Mass balance calculations using CheMin results and bulk elemental measurements by the Alpha Particle X-ray Spectrometer suggest the amorphous component in Gale crater is variably enriched in Si, Fe, and S [e.g., 7,8]. The compositions are not consistent with pure volcanic glass, indicating water must have been involved in the formation of amorphous materials in Gale crater. We seek to better constrain the conditions under which amorphous materials on Mars formed by studying the composition and short-range atomic order of amorphous materials in terrestrial analog environments via XRD and transmission electron microscopy (TEM).

E B Rampe↗
NASA NTRS1999

Measuring the Chemical Potential of the Martian Regolith to Generate and Sustain Life

A critical component for identifying chemical biosignatures is the ability to assess in-situ the potential of an aqueous geochemical environment to generate and sustain life. On Mars or other solar bodies, in-situ chemical characterization could provide evidence as to whether the chemical composition of the regolith or evaporites in suspected ancient water bodies have been biologically influenced or possess the chemical parameters within which life may have existed, or may still exist. A variety of analytical techniques have been proposed for use in detecting and identify signatures of past or present life. These techniques fall into two groups; visual observation with instruments such as cameras or optical/atomic-force microscopes; or elemental chemical analysis with such instruments as X-ray fluorescence (XRF) and diffraction (XRD), a-proton backscatter (APX), y-ray, Mossbauer, Raman, IR, UV/VIS spectroscopies, gas chromatography (GC), or mass spectrometry (MS). Direct observation of an identifiable lifeform by the first set of instruments in a single sample is highly unlikely, especially for extinct organisms or on the surface. The later instruments can provide vital data as to the elemental mineralogy and geological history of the planet, but are highly inadequate for understanding the chemistry of the planet in terms of indigenous life or interactions with human explorers. Techniques such as XRD, XRF, and APX, provide elemental composition at high limits of detection. Some of this data can be extrapolated or interpolated to provide chemical parameters such as oxidation state or composition. Gas chromatography (GC) without standards and non-specific detectors, has little chance of identifying a mixture of unknown components. Combined with GC or by itself, mass spectrometry (MS) can provide identification of compounds, but in both cases the sample must be appropriately prepared for accurate and reliable analysis. Life as we know it, and probably identify it as such, requires an aqueous environment. Deciphering die chemical speciation of this aqueous environment is the key to recognizing therein the biosignatures of any extinct or present life forms. Identifying the soluble (ionic and nonionic) components by reacting a currently dormant environment can provide a "picture" of the thermodynamics and chemical components of a possibly bioactive environment. The only devices which can provide such information are electrochemical sensors based on the potentiometric ion selective electrodes (ISEs) and on dynamic techniques such as cyclic voltammetry (CV) and stripping voltammetry (SV). Such an array of devices can provide not only the chemical composition of a water-soluble Martian soil sample, but also several other vital chemical parameters such as pH, conductivity, redox potential, and dissolved gases. To address these issues we have been investigating the possible use of an electrochemically-based ion sensor array as a new integrated approach to quantitative analytical and chemometric electrochemical measurements. The sensor array will consist of specific and semispecific ion selective and amperometric transducers, which can simultaneously and continuously identify and semiquantitatively determine over 50 organic and inorganic analytes in water-based environments. Several individual sensors, based on the same principle, have been flight-tested and have been installed as part of the MECA instrumentation on the Mars 2001 Lander for in-situ analyses. However, the microfabrication, integration and multiplexing of such a large number of these sensors on a single substrate have not been previously attempted.

Kounaves, S. P.↗
NASA NTRSDate not supplied

Magma-Sediment Interaction Induced Alteration Mineralogy on Mars: Detectability and Analytical Method Comparison Using the Curtis Sandstone as A Terrestrial Analog

Basaltic magmatism is a ubiquitous feature of the Martian crust, and would have interacted with sediments and fluids through the geologic history of Mars to potentially produce higher temperature hydrothermal systems , and contact metamorphic rocks. On Earth, comparable hydrothermal systems represent habitable environments, which can be used as an analog for Mars. Nevertheless, evidence of aforementioned hydrothermal systems on Mars has remained elusive, despite the efforts of both orbital and in-situ analyses. Limited low grade metamorphic minerals typically indicative of hydrothermal systems (prehnite, zeolites, serpentine) have been detected in the Martian crust, though the detections are typically isolated occurrences, and do not necessarily indicate an in-place metamorphic sequence. It is possible that orbital spectroscopy alone is not capable of detecting such an alteration front, with higher resolution in-situ analyses being required to detect the changes in mineralogy and species of alteration minerals associated with magma-sediment interaction. To constrain this, we have investigated a terrestrial analog on the Colorado Plateau, USA, where a mafic dike intrudes a quartz areinite of the Jurassic Curtis Sandstone. The investigation was carried out using Mars relevant instruments: Visible to Near-Infrared (VNIR) spectroscopy analogous to orbital spectroscopy, and X-ray Diffraction (XRD) analogous to CheMin on Mars Sample Laboratory Curiosity. While quartz sandstones have not been, and are unlikely to be, detected on Mars, the relatively mineralogically uniform Curtis Sandstone serves as analog here as it avoids complications of multiple mineral systems or significant element exchange with the surrounding area.

J R Crandall↗
DOE OSTI2025

In-Situ Synchrotron X-Ray Diffraction of Ultrasonic Microstructural Refinement During Solidification in a Commercial Al–Si–Mg Alloy

This study reports the first use of in-situ synchrotron X-ray diffraction (SXRD) to study the effects of ultrasonic melt processing (USMP) on phase and grain size evolution during solidification in a commercial Al–Si–Mg casting alloy. USMP is a technique that, when applied to aluminum as it solidifies, can be used to refine the local microstructure of large-scale castings. Analysis of the in-situ SXRD data to estimate the average grain size of primary α-Al grains during USMP demonstrates that USMP slows the growth rate of α-Al grains and reduces grain size by 36 pct. Furthermore, there is also evidence that USMP causes the primary α-Al grains to move relative to the X-ray beam; such motion increases the probability of primary α-Al grains colliding and fragmenting. This movement becomes constrained at the onset of the Al–Si binary eutectic, suggesting that USMP ceases to effectively refine the microstructure once the Al–Si binary eutectic begins to form. Complementary laboratory-scale X-ray diffraction (XRD) data were used to correlate the lattice parameters of the α-Al and Si (D-A4) phases with temperature to estimate cooling rate during solidification. Thus, this study can guide the design of novel castings with spatially distributed fine-grained regions produced using local ultrasonic processing.

Aluminum Alloys↗
DOE OSTI2026

Influence of thermal treatment on structure and catalytic performance of ceria-zirconia supported copper oxide (CuO x /Ce y Zr 1-y O 2 ) catalysts for CO oxidation

Copper oxide (CuO x ) supported on ceria-zirconia (Ce y Zr 1-y O 2 , y = 1.0, 0.5, 0.0) catalysts were investigated to elucidate the effects of thermal treatment on their physicochemical properties and catalytic performance in carbon monoxide (CO) oxidation. Here, the catalysts were synthesized via a one-pot chemical vapor deposition (OP-CVD) method at 700˚C and 900˚C with controlled Cu loading. Characterization techniques, including synchrotron X-ray diffraction (S-XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma spectroscopy (ICP), and N 2 adsorption-desorption, were implemented to probe the crystalline structure, molecular and electronic structure, oxygen vacancies, specific surface area (SSA) and metal loading. CO oxidation was chosen as a model reaction to explore the structure-catalytic performance relationship. A ∼100% CO conversion was achieved at < 150˚C, particularly with the CuO x /CeO 2 catalyst calcined at 700˚C. In contrast, calcination at 900˚C caused a ∼90% decrease in SSA and a ∼24% increase in T 50 . Activity tests revealed that increasing ZrO 2 content lowered CO oxidation activity despite generating more defect sites. In-situ measurement of the 700 °C calcined samples revealed the presence of stable and unstable defects in CuO x /Ce 0.5 Zr 0.5 O 2 and CeO 2 respectively, which play a key role in the activity of the catalysts. The results highlight that catalytic performance is closely related to the SSA. Furthermore, an optimum calcination temperature favor significant oxygen vacancy formation with required CuO x -support interactions, enhancing redox properties and catalytic performance.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Elucidating the factors controlling the methanol synthesis from CO 2 on ZnPd-ZnO/TiO 2 catalysts prepared by direct/inverse impregnation

The direct hydrogenation of CO 2 to methanol over supported ZnPd intermetallic catalysts remains a challenge due to the complex nature of the active sites, which are highly dependent on both the dispersion of ZnPd intermetallics and their proximity to ZnO. This study investigates the effect of the Pd and Zn incorporation order on methanol synthesis over TiO 2 -supported ZnPd catalysts. Catalysts were prepared via direct (Pd/Zn), inverse (Zn/Pd), and co-impregnation (Pd+Zn) methods using anatase TiO 2 as the support. Comprehensive characterization by XRD, HRTEM, CO-DRIFTS and XPS revealed that the formation of small and crystalline intermetallic β-ZnPd particles and their interaction with ZnO/ZnO x depends on the sequence of Pd and Zn incorporation. It was found that, under the reaction conditions, the ZnO x species plays a critical role in facilitating the formation of the intermetallic ZnPd through the interactions between Pd and ZnO x . In addition, ZnO x species have also been shown to modulate key catalytic properties, such as CO 2 activation and methanol selectivity. Specifically, the ZnPd/Pd surface ratio, determined by Pd dispersion and proximity to ZnO/ZnO x , was shown to determine the methanol production from CO 2 directly or via a CO intermediate. The Pd/Zn catalyst showed superior selectivity due to the in-situ formation of intermetallic species facilitated by Pd-ZnO x interactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRSDate not supplied

Thermochemical Interactions of Yttria-Stabilized Zirconia and Molten Lunar Regolith Simulants

Oxygen produced from lunar resources through in-situ resource utilization (ISRU) is critical to maintaining a permanent human presence on the lunar surface. Molten regolith electrolysis and carbothermal reduction are two promising ISRU techniques for generating oxygen directly from lunar regolith, which is primarily a mixture of oxide minerals; however, both processes require operating temperatures of 1600C to melt lunar regolith and dissociate the molten oxides. These conditions limit the use of many oxide refractory materials, such as Al2O3 and MgO, due to rapid degradation resulting from reactions between the refractory materials and molten lunar regolith. Yttria-stabilized zirconia (YSZ) is a promising refractory oxide to provide containment of molten regolith while demonstrating limited reactivity. This work focuses on corrosion studies of YSZ powders and dense YSZ crucibles in contact with molten lunar mare and highlands regolith simulants at 1600C. The interactions between YSZ and molten regolith are characterized using SEM/EDS, XRD, and EBSD with an emphasis on elemental and microstructural analysis to assess reactivity and degradation of YSZ. Due to lunar regolith’s similar composition to calcium-magnesium-aluminosilicates (CMAS) and YSZ’s usage as a thermal barrier coating, these interactions can serve to inform YSZ/CMAS behavior by simulating cases of elevated CMAS/YSZ ratios and for higher than intended gas turbine temperatures.

Kevin Yu↗
NASA NTRS2024

Thermochemical Interactions Between Yttria-Stabilized Zirconia and Molten Lunar Regolith Simulants

Oxygen produced through in-situ resource utilization (ISRU) is critical to maintaining a permanent human presence on the lunar surface. Molten regolith electrolysis and carbothermal reduction are two promising ISRU techniques for generating oxygen directly from lunar regolith, which is primarily a mixture of oxide minerals; however, both processes require operating temperatures of 1600 C to melt lunar regolith and dissociate the molten oxides. These conditions limit the use of many oxide refractory materials, such as Al2O3 and MgO, due to rapid degradation resulting from reactions between the refractory materials and molten lunar regolith. Yttria-stabilized zirconia (YSZ) is shown here to be a promising refractory oxide to provide containment of molten regolith while demonstrating limited reactivity. This work focuses on corrosion studies of YSZ powders and dense YSZ crucibles in contact with molten lunar maria and highlands regolith simulants at 1600 C. The interactions between YSZ and molten regolith are characterized using SEM/EDS, XRD, and EBSD. A FactSage thermochemical model is created to compare with the experimental results. These combined analyses suggest that lunar maria regolith will degrade YSZ faster than lunar highlands regolith due to the lower viscosity of the maria regolith. The feasibility of long-term molten regolith containment with YSZ is discussed based on the YSZ powder and crucible results.

Kevin Yu↗
NASA NTRS2002

A Miniature Mineralogical Instrument for In-Situ Characterization of Ices and Hydrous Minerals at the Lunar Poles

Lunar missions over the past few years have provided new evidence that water may be present at the lunar poles in the form of cold-trapped ice deposits, thereby rekindling interest in sampling the polar regions. Robotic landers fitted with mineralogical instrumentation for in-situ analyses could provide unequivocal answers on the presence of crystalline water ice and/or hydrous minerals at the lunar poles. Data from Lunar Prospector suggest that any surface exploration of the lunar poles should include the capability to drill to depths of more than 40 cm. Limited data on the lunar geotherm indicate temperatures of approximately 245-255 K at regolith depths of 40 cm, within a range where water may exist in the liquid state as brine. A relevant terrestrial analog occurs in Antarctica, where the zeolite mineral chabazite has been found at the boundary between ice-free and ice-cemented regolith horizons, and precipitation from a regolith brine is indicated. Soluble halogens and sulfur in the lunar regolith could provide comparable brine chemistry in an analogous setting. Regolith samples collected by a drilling device could be readily analyzed by CheMin, a mineralogical instrument that combines X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques to simultaneously characterize the chemical and mineralogical compositions of granular or powdered samples. CheMin can unambiguously determine not only the presence of hydrous alteration phases such as clays or zeolites, but it can also identify the structural variants or types of clay or zeolite present (e.g., well-ordered versus poorly ordered smectite; chabazite versus phillipsite). In addition, CheMin can readily measure the abundances of key elements that may occur in lunar minerals (Na, Mg, Al, Si, K, Ca, Fe) as well as the likely constituents of lunar brines (F, Cl, S). Finally, if coring and analysis are done during the lunar night or in permanent shadow, CheMin can provide information on the chemistry and structure of any crystalline ices that might occur in the regolith samples.

Sarrazin, P.↗
NASA NTRS2014

Amorphous Phases on the Surface of Mars

Both primary (volcanic/impact glasses) and secondary (opal/silica, allophane, hisingerite, npOx, S-bearing) amorphous phases appear to be major components of martian surface materials based on orbital and in-situ measurements. A key observation is that whereas regional/global scale amorphous components include altered glass and npOx, local scale amorphous phases include hydrated silica/opal. This suggests widespread alteration at low water-to-rock ratios, perhaps due to snow/ice melt with variable pH, and localized alteration at high water-to-rock ratios. Orbital and in-situ measurements of the regional/global amorphous component on Mars suggests that it is made up of at least three phases: npOx, amorphous silicate (likely altered glass), and an amorphous S-bearing phase. Fundamental questions regarding the composition and the formation of the regional/global amorphous component(s) still remain: Do the phases form locally or have they been homogenized through aeolian activity and derived from the global dust? Is the parent glass volcanic, impact, or both? Are the phases separate or intimately mixed (e.g., as in palagonite)? When did the amorphous phases form? To address the question of source (local and/or global), we need to look for variations in the different phases within the amorphous component through continued modeling of the chemical composition of the amorphous phases in samples from Gale using CheMin and APXS data. If we find variations (e.g., a lack of or enrichment in amorphous silicate in some samples), this may imply a local source for some phases. Furthermore, the chemical composition of the weathering products may give insight into the formation mechanisms of the parent glass (e.g., impact glasses contain higher Al and lower Si [30], so we might expect allophane as a weathering product of impact glass). To address the question of whether these phases are separate or intimately mixed, we need to do laboratory studies of naturally altered samples made up of mixed phases (e.g., palagonite) and synthetic single phases to determine their short-range order structures and calculate their XRD patterns to use in models of CheMin data. Finally, to address the timing of the alteration, we need to study rocks on the martian surface of different ages that may contain glass (volcanic or impact) with MSL and future rovers to better understand how glass alters on the martian surface, if that alteration mechanism is universal, and if alteration spans across long periods of time or if there is a time past which unaltered glass remains.

Rampe, E. B.↗
DOE OSTI2026

High hardness and oxidation-resistant Cr-containing medium entropy ZrTaW diboride

This study reports the successful synthesis of a Cr-containing (Zr 0.30 Ta 0.34 Cr 0.06 W 0.30 )B 2 medium-entropy boride (MEB) via an in-situ reactive borothermal reduction route from oxide precursors. High-energy ball milling was employed to homogenize the precursor mixture prior to reactive densification. X-ray diffraction confirmed the formation of a predominantly AlB₂-type hexagonal diboride structure together with a secondary (W X , M 1-X )B monoboride phase. Microstructural characterization revealed compositional heterogeneity and localized W-rich regions associated with the secondary phase. The synthesized medium-entropy boride exhibited enhanced mechanical properties, which are attributed to lattice distortion and solid-solution strengthening effects. Thermogravimetric analysis revealed complex multistage oxidation behavior, and the oxidation resistance was compared with conventional ultra-high-temperature diborides. The results demonstrate the strong relationship between oxide-derived processing, compositional complexity, phase evolution, and oxidation behavior, highlighting the potential of medium-entropy borides for high-temperature structural applications

36 MATERIALS SCIENCE↗
DOE OSTI2026

Discovery of a new phase transition and high-valent redox mechanism in Fe-substituted Na 2 Mn 3 O 7

Sodium-ion batteries are a promising lower-cost alternative to lithium-ion batteries, but further improvements in electrochemical performance are required. One strategy to increase capacity is to enable reversible high-valent cationic and anionic redox in layered cathode materials; however, this is typically accompanied by structural degradation. Here, in this study, we elucidate the mechanism by which Fe-doped Na 2 Mn 3 O 7 , featuring ordered transition metal-vacancies, achieves reversible high-valent redox. Using Mössbauer spectroscopy, soft X-ray absorption spectroscopy (XAS), and in-situ hard XAS, we demonstrate reversible high-valent cationic redox involving both Fe and Mn while in-situ Raman confirms the absence of local structural degradation associated with oxygen redox. Combining in-situ X-ray diffraction with theoretical calculations, we further identify a previously unreported global phase transition from the $\bar{P1}$ to the $P2_1/c$ space group during electrochemical cycling and develop a physical model describing this structural evolution. These results provide insights for structurally stable layered sodium transition metal oxide cathodes with reversible high-valent redox.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Enhancing low-temperature sintering in the MgO-LiF system: Mechanistic insights

In the present article, we provide compelling evidence that minor (1 wt%) additions of micron and nanometre-sized LiF particles in MgO decompose leading to free Li diffusing into MgO surfaces enhancing vacancy production during direct current sintering. The addition of nanometre-sized LiF particles leads to a > 500 °C reduction in the sintering temperature and over 99 % theoretical density of final consolidated compacts. Correlating differential scanning calorimetry with in-situ x-ray diffraction, together with Schottky calculations, post sintering electron microscopy and laser induced breakdown spectroscopy, we uncover critical insights into this impressive reduction in sintering temperature. Our quantitative analysis reveals that MgO and LiF interact at low temperatures with the diffusion of Li into the surface of MgO particles due to the intrinsic structural disorder of the LiF and MgO crystallites. Nanometre-sized LiF particles were found to react the most at low temperatures due to their increased structural disorder. Our multimodal characterization points to a Li-promoted densification and sintering mechanism. This impressive reduction in sintering temperature can be harnessed to promote low-temperature fabrication of MgO-based composites for technological applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Defect-Driven Redox Interplay on Anatase TiO 2 : Surface-Structure Dependent Activation for CO 2 Hydrogenation Catalysis

Titanium dioxide (TiO 2 ) is one of the most extensively studied oxides as an active catalyst or catalyst support, particularly in energy and environmental applications, but the atomistic mechanisms governing its dynamic response to reactive environments and their correlation to reactivity remain largely elusive. Using in situ environmental transmission electron microscopy (ETEM), synchrotron X-ray diffraction (XRD), ambient-pressure X-ray photoelectron spectroscopy (AP-XPS), temperature-programmed reduction (TPR), reactivity measurements, and theoretical modeling, we reveal the dynamic interplay between oxygen loss and replenishment of anatase TiO 2 under varying reactive conditions. Under H 2 exposure, anatase TiO 2 undergoes surface reduction via lattice oxygen loss, forming Ti 3 O 5 . In contrast, CO 2 exposure induces oxygen replenishment, reversing stoichiometry. In mixed H2/CO 2 environments, the reverse water–gas shift (RWGS) reaction proceeds selectively on stepped and high-indexed TiO 2 surfaces, whereas the thermodynamically stable TiO 2 (101) surface remains inactive and intact. Critically, H 2 pretreatment generates oxygen vacancies on TiO 2 (101), transforming it into an active Ti 3 O 5 or defect-rich surface that catalyzes RWGS. By correlating surface structure, defect dynamics, and gas-phase interactions, this work deciphers the competition between H 2 -driven reduction and CO 2 -driven oxidation pathways at the atomic scale. Furthermore, these insights establish defect engineering as a strategic lever to activate inert TiO 2 facets, advancing the design of adaptive catalysts for sustainable fuel synthesis technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Fe-single atom catalysts facilitate fast electron transfer with MoS 2 /SnS 2 cathodes in lithium–sulfur batteries

Lithium–sulfur batteries (LSBs) emerge as promising next-generation energy storage systems offering cost-effectiveness, environmental friendliness, and high theoretical energy density. The practical implementation of LSBs faces significant hindrances due to the shuttle effect and sluggish redox reactions. To address these challenges, single-atom catalyst (SAC) based combination materials from d-block elements can offer increased active catalytic sites, rapid charge transfer, accelerated electron migration, and fast sulfur redox conversion kinetics of lithium polysulfides (LiPSs). In this study, we fabricated three different LSB cathodes: pure S, S@MoS 2 /SnS 2 , and S@Fe–MoS 2 /SnS 2 . These cathodes were then used to explore the cycle life, capacity, rate capability, and redox kinetic reactions of LiPSs while assessing the influence of Fe-SACs on their performance. As a result, LSBs with S@Fe–MoS 2 /SnS 2 cathodes demonstrate an extended cycle life of 1000 cycles at a C-rate of 0.2C, maintaining a capacity close to 500 mA h g −1 , the highest initial discharge capacity of 1622 mA h g −1 and 1066 mA h g −1 at 0.05C and 0.2C, and excellent rate capabilities of 708 mA h g −1 and 558 mA h g −1 at 1C and 2C, respectively. The synergistic effect of the Fe-SAC-based combination cathode (S@Fe–MoS 2 /SnS 2 ) creates plentiful adsorptive and highly active catalytic sites, resulting in substantially enhanced capacity for adsorbing soluble long-chain LiPSs. This facilitates ultra-fast redox kinetics, surpassing the performance of the S@MoS 2 /SnS 2 and pure S cathodes. In the ex situ analysis, results from powder X-ray diffraction (XRD) to observe the new phase, soft X-ray absorption spectroscopy (XAS) to investigate the electronic structure, and hard X-ray photoelectron microscopy (HAXPES) with different energies (900 eV, 2000 eV, and 6000 eV) to track the chemical-state evolution of Fe-SACs in MoS 2 /SnS 2 cathodes displayed notable electrochemical reversibility involving S 8 ⇄ LiPSs ⇄ Li 2 S conversion even after 1000 cycles. Additionally, in situ, operando Raman analysis can unveil a novel catalytic mechanism of Fe-SACs in MoS 2 /SnS 2 “facilitating rapid electron transfer” during the discharge and charge processes of LSBs involving the conversion of S 8 ⇄ long-chain LiPSs ⇄ Li 2 S 2 /Li 2 S. This study elucidates the working mechanism of Fe-SAC cathodes, offering insights into overcoming the shuttle effect and facilitating sulfur redox kinetics to advance commercial LSBs.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In-Situ and Ex-Situ Studies on the Morphology Changes of Polymer Pipeline Materials for Use in Hydrogen Gas Environments

The US natural gas infrastructure is a national asset that could be used to deliver hydrogen and hydrogen blends of natural gas as a pathway to reduce carbon emissions. The distribution system comprises nearly 50% plastic pipe composed of medium- and high-density polyethylene materials (MDPE and HDPE). While these materials perform adequately for natural gas, research on their hydrogen compatibility is essential to understand if any immediate and long-term risks are associated with hydrogen addition. The Blended Gas CRADA, a HyBlend project, has established a comprehensive test method for evaluating MDPE and HDPE of various plastic resin compositions of pipeline material in pure hydrogen and 20% hydrogen/80% methane blends. Both in-situ and ex-situ measurements were performed to capture hydrogen-induced changes in the polyethylene material's crystalline, amorphous and their interphase regions. We investigated MDPE and HDPE pipeline materials made from different polymer resin systems to evaluate the effects of hydrogen gas. The materials were characterized by their density, diffusion coefficient, free volume ratio, and degree of crystallinity. Various advanced characterization methods, including in situ NMR, ex situ XRD, ex situ DSC, and ex situ TDA, were used to analyze the effects of changes in crystalline, amorphous, and interphase regions due to gas exposure. Time-dependent post-decompression quasi-static tensile tests were conducted to explore the effects of gas exposure time on the mechanical behavior of the pipe materials. This work will highlight the time sensitivities during and after gas exposure. The correlation between gas-induced polyethylene morphology changes and the associated material performance will be addressed for the intended applications. These studies will show that polyethylene resin composition and material exposure are important factors when considering whether hydrogen gas affects pipeline materials positively or negatively.

Simmons, Kevin L.↗
NASA NTRS2003

In-SITU Raman Spectroscopy of Single Microparticle Li-Intercalation Electrodes

Modifications in the vibrational properties of a single microparticle of LiMn2O4 induced by extraction and subsequent injection of Li(+) into the lattice have been monitored in situ via simultaneous acquisition of Raman scattering spectra and cyclic voltammetry data in 1M LiC1O4 solutions in ethylene carbonate (EC):diethyl carbonate (DEC) mixtures (1:1 by volume). Statistical analyses of the spectra in the range 15 < SOD < 45%, where SOD represents the state of discharge (in percent) of the nominally fully charged material, i.e. lambda-MnO2, were found to be consistent with the coexistence of two distinct phases of lithiated metal oxide in agreement with information derived from in situ X-ray diffraction (XRD) measurements involving more conventional battery-type electrodes.

Dokko, Kaoru↗
NASA NTRS2004

Lunar and Planetary Science XXXV: Missions and Instruments: Hopes and Hope Fulfilled

The titles in this section include: 1) Mars Global Surveyor Mars Orbiter Camera in the Extended Mission: The MOC Toolkit; 2) Mars Odyssey THEMIS-VIS Calibration; 3) Early Science Operations and Results from the ESA Mars Express Mission: Focus on Imaging and Spectral Mapping; 4) The Mars Express/NASA Project at JPL; 5) Beagle 2: Mission to Mars - Current Status; 6) The Beagle 2 Microscope; 7) Mars Environmental Chamber for Dynamic Dust Deposition and Statics Analysis; 8) Locating Targets for CRISM Based on Surface Morphology and Interpretation of THEMIS Data; 9) The Phoenix Mission to Mars; 10) First Studies of Possible Landing Sites for the Phoenix Mars Scout Mission Using the BMST; 11) The 2009 Mars Telecommunications Orbiter; 12) The Aurora Exploration Program - The ExoMars Mission; 13) Electron-induced Luminescence and X-Ray Spectrometer (ELXS) System Development; 14) Remote-Raman and Micro-Raman Studies of Solid CO2, CH4, Gas Hydrates and Ice; 15) The Compact Microimaging Spectrometer (CMIS): A New Tool for In-Situ Planetary Science; 16) Preliminary Results of a New Type of Surface Property Measurement Ideal for a Future Mars Rover Mission; 17) Electrodynamic Dust Shield for Solar Panels on Mars; 18) Sensor Web for Spatio-Temporal Monitoring of a Hydrological Environment; 19) Field Testing of an In-Situ Neutron Spectrometer for Planetary Exploration: First Results; 20) A Miniature Solid-State Spectrometer for Space Applications - Field Tests; 21) Application of Laser Induced Breakdown Spectroscopy (LIBS) to Mars Polar Exploration: LIBS Analysis of Water Ice and Water Ice/Soil Mixtures; 22) LIBS Analysis of Geological Samples at Low Pressures: Application to Mars, the Moon, and Asteroids; 23) In-Situ 1-D and 2-D Mapping of Soil Core and Rock Samples Using the LIBS Long Spark; 24) Rocks Analysis at Stand Off Distance by LIBS in Martian Conditions; 25) Evaluation of a Compact Spectrograph/Detection System for a LIBS Instrument for In-Situ and Stand-Off Detection; 26) Analysis of Organic Compounds in Mars Analog Samples; 27) Report of the Organic Contamination Science Steering Group; 28) The Water-Wheel IR (WIR) - A Contact Survey Experiment for Water and Carbonates on Mars; 29) Mid-IR Fiber Optic Probe for In Situ Water Detection and Characterization; 30) Effects of Subsurface Sampling & Processing on Martian Simulant Containing Varying Quantities of Water; 31) The Subsurface Ice Probe (SIPR): A Low-Power Thermal Probe for the Martian Polar Layered Deposits; 32) Deploying Ground Penetrating Radar in Planetary Analog Sites to Evaluate Potential Instrument Capabilities on Future Mars Missions; 33) Evaluation of Rock Powdering Methods to Obtain Fine-grained Samples for CHEMIN, a Combined XRD/XRF Instrument; 34) Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation; 35) A New Celestial Navigation Method for Mars Landers; 36) Mars Mineral Spectroscopy Web Site: A Resource for Remote Planetary Spectroscopy.

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