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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Direct visualization of radiation-induced transformations at alkali halide–air interfaces

Radiation driven reactions at mineral/air interfaces are important to the chemistry of the atmosphere, but experimental constraints (e.g. simultaneous irradiation, in situ observation, and environmental control) leave process understanding incomplete. Using a custom atomic force microscope equipped with an integrated X-ray source, transformation of potassium bromide surfaces to potassium nitrate by air radiolysis species was followed directly in situ at the nanoscale. Radiolysis initiates dynamic step edge dissolution, surface composition evolution, and ultimately nucleation and heteroepitaxial growth of potassium nitrate crystallites mediated by surface diffusion at rates controlled by adsorbed water. Finally, in contrast to in situ electron microscopy and synchrotron-based imaging techniques where high radiation doses are intrinsic, our approach illustrates the value of decoupling irradiation and the basis of observation.

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

Molecular-level understanding of metal ion retention in clay-rich materials

Clay minerals retain or adsorb metal ions in the Earth’s critical zone. Rocks, sediments and soils rich in clay minerals can concentrate rare earth elements (REEs) in ion adsorption-type deposits (IADs) and are similarly effective at metallic contaminant remediation. However, the molecular-scale chemical and physical mechanisms of metal ion retention remain only partly understood. Here, we describe the nature, location and energy requirements of metal retention at clay mineral surfaces. Retention originates mainly from electrostatic interactions during cation exchange at low pH and chemical bonding in surface complexation and precipitation at neutral and high pH. Surface complexation can induce surface redox reactions and precipitation mechanisms including neoformation of clay mineral layered structures. In IADs, outer-sphere adsorption is the major retention mechanism of REE ions. By contrast, the use of clay minerals in pollution control relies on various mechanisms that can coexist, including cation exchange, surface complexation and nucleation growth. To more effectively leverage clay mineral–metal interactions in resource recovery and contaminant remediation, complex mechanisms such as surface precipitation and redox reactions must be better understood; for instance, by utilizing advances in quantum mechanical calculations, close combination between synchrotron and simulation techniques, and upscaling of molecular-level information in macroscopic thermokinetic predictive models.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Revealing pressure-driven structural transitions in the hybrid improper ferroelectric Sr 3 Sn 2 O 7

In this work, we combine diamond anvil cell techniques and synchrotron-based infrared spectroscopy with a detailed symmetry analysis and lattice dynamics calculations to uncover a series of pressure induced structural phase transitions in the hybrid improper ferroelectric Sr 3 Sn 2 O 7 . The microscopic character of each high pressure phase is determined by comparing the measured spectrum with the predicted vibrational patterns of several related but distinct candidate space groups. Our analysis reveals a sequence of compression-induced transitions from A2 1 am ↔ Pnab ↔ Acaa ↔ I4/mmm at room temperature. Remarkably, this space group progression matches the sequence of temperature-dependent structural transitions observed in Sr 3 Sn 2 O 7 between 77 and 1000 K. Other hybrid improper ferroelectrics display a similar set of transitions, suggesting that pressure and probably strain will be very effective tuning parameters for this entire class of materials.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Seasonal Zinc Storage and a Strategy for Its Use in Buds of Fruit Trees

Bud dormancy allows deciduous perennial plants to rapidly grow following seasonal cold conditions. Although many studies have examined the hormonal regulation of bud growth, the role of nutrients remains unclear. Insufficient accumulation of the key micronutrient zinc (Zn) in dormant buds affects the vegetative and reproductive growth of perennial plants during the subsequent year, requiring the application of Zn fertilizers in orchard management to avoid growth defects in fruit trees. However, the mechanisms of seasonal Zn homeostasis in perennial plants remain poorly understood. Here, we provide new insights into Zn distribution and speciation within reproductive and vegetative buds of apple (Malus domestica) and four other deciduous fruit trees (peach [Amygdalus persica], grape [Vitis vinifera], pistachio [Pistacia vera], and blueberry [Vaccinium spp.]) using microscopic and spectroscopic characterization techniques comprising synchrotron-based x-ray fluorescence and x-ray absorption near-edge-structure analyses. By establishing a link between bud development and Zn distribution, we identified the following important steps of Zn storage and use in deciduous plants: Zn is preferentially deposited in the stem nodes subtending apical and axillary buds; Zn may then be sequestered as Zn-phytate prior to dormancy; in spring, Zn effectively releases for use during budbreak and subsequent meristematic growth. The mechanisms of Zn homeostasis during the seasonal cycles of plant growth and dormancy described here will contribute to improving orchard management, and to selection and breeding of deciduous perennial species.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Isoxazole-Based Electrolytes for Lithium Metal Protection and Lithium-Sulfurized Polyacrylonitrile (SPAN) Battery Operating at Low Temperature

A new electrolyte system using isoxazole as the salt dissolving solvent has been developed and studied for lithium metal batteries. By using fluoroethylene carbonate (FEC) as an additive and 1,1,2,2-tetrafluoroethyl-2,2,3,3-tetrafluoropropyl ether (TTE) as a diluent for localized high concentration electrolyte (LHCE), isoxazole-based electrolytes were successfully implemented in lithium metal batteries, demonstrating excellent lithium metal protection capability. Utilizing several advanced characterization techniques (including synchrotron-based X-ray absorption spectroscopy and photoelectron spectroscopy), the solid electrolyte interphase (SEI) formed on the Li-metal anode after employing these electrolytes was thoroughly investigated. The high ionic conductivity of isoxazole at low temperature and the low impedance of SEI formed in LHCE significantly improved the low-temperature performance of Li-sulfurized polyacrylonitrile (SPAN) batteries, delivering 273.8 mAh g −1 capacity at −30 °C with 99.85% capacity retention after 50 cycles.

25 ENERGY STORAGE↗
DOE OSTI2023

The iron spin transition of deep nitrogen-bearing mineral Fe3N1.2 at high pressure

Abstract Nitrogen is an essential element for life, one of the most abundant volatiles in the atmosphere, and an important component in the Earth’s interior, where iron nitride is an essential host of deep nitrogen. Here, we investigate the pressure-induced electronic spin-pairing transition of iron in siderazot (Fe3N1.2) at pressures up to 45.8 GPa at room temperature, using diamond-anvil cell techniques coupled with synchrotron X-ray emission spectroscopy. The integrated intensity of the satellite emission peak (K′β) decreases upon compression but remains unchanged at pressures greater than 30.5 GPa. In other words, the high-spin to low-spin transition of iron in Fe3N1.2 starts immediately at very low pressures and completes at ~30.5 GPa. The iron spin transition completion pressures increase with the nitrogen concentration of hexagonal close-packed iron nitrides (i.e., Fe3N1.2, Fe7N3, and Fe2N). Moreover, the identity and concentration of light elements in binary iron-rich compounds such as Fe3N, Fe3C, Fe3P, Fe3S, Fe7C3, and Fe7N3, together with their crystal structure, could affect the iron spin transition pressures. The spin transition of iron-rich alloys could alter the bonding nature and the physical properties, including the thermal and electrical conductivity, thereby influencing the thermal state and evolution of planetary interiors.

Geochemistry & Geophysics↗
DOE OSTI2023

Temperature-induced densification in compressed basaltic glass revealed by in-situ ultrasonic measurements

Abstract Acoustic velocities of a model basalt glass (64 mol% CaMgSi2O6 + 36 mol% CaAl2Si2O8) were measured along different pressure-temperature (P-T) paths. One set of experiments involved isothermal compression-decompression cycles, performed at temperatures of 300, 641, 823, and 1006 K and pressures up to 12.2 GPa. The other set of experiments involved constant-load heating-cooling cycles at temperatures up to 823 K and pressures up to 7.5 GPa. Both sets of experiments were performed in a multi-anvil apparatus using a synchrotron-based ultrasonic technique. Our results show that the glass compressed isothermally at 300 K (cold-compression) displays anomalously decreasing compressional (VP) and shear (VS) wave velocities with increasing pressure until ~8 GPa. Beyond 8 GPa, both VP and VS start to increase sharply with pressure and irreversible densification of the glass occurred, producing large hysteresis loops of velocities upon decompression. However, for the glass compressed isothermally at increasingly higher temperatures (hot-compression), the velocity minima gradually shift to lower pressures. At temperature close to the glass transition temperature Tg, the velocity minima disappear completely, displaying a monotonic increase of velocities during compression and higher VP and VS during decompression. In addition, constant-load heating-cooling experiments show that velocities generally decrease slightly with increasing temperature, but start to increase once heated above a threshold temperature (~650 K). During cooling the velocities increase almost linearly with decreasing temperature, resulting in higher velocities (~1.5–2.5% higher) when returned to 300 K. This implies that a temperature-induced densification may have occurred in the glass at high pressures. Raman spectra on recovered samples show that the hot-compressed and high-P heated glasses contain distinctly densified and depolymerized structural signatures compared to the initial glass and the cold-compressed glass below the velocity transition pressure PT (~8 GPa). Such densification may be attributed to the breaking of bridging oxygen bonds and compaction in the intermediate-range structure. Our results demonstrate that temperature can facilitate glass densification at high pressures and point out the importance of P-T history in understanding the elastic properties of silicate glasses. Comparison with melt velocity suggests that hot-compressed glasses may better resemble the pressure dependence of velocity of silicate melts than cold-compressed glasses, but still show significantly higher velocities than melts. If the abnormal acoustic behaviors of cold-compressed glasses were used to constrain melt fractions in the mantle low-velocity regions, the melt fractions needed to explain a given velocity reduction would be significantly underestimated at high pressures.

Geochemistry & Geophysics↗
DOE OSTI2023

Vibronic Relaxation Pathways in Molecular Spin Qubit Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O under Pressure

In order to explore how spectral sparsity and vibronic decoherence pathways can be controlled in a model qubit system with atomic clock transitions, we combined diamond anvil cell techniques with synchrotron-based far infrared spectroscopy and first-principles calculations to reveal the vibrational response of Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O under compression. Because the hole in the phonon density of states acts to reduce the overlap between the phonons and f manifold excitations in this system, we postulated that pressure might move the HoO 4 rocking, bending, and asymmetric stretching modes that couple with the M J = ±5, ±2, and ±7 levels out of resonance, reducing their interactions and minimizing decoherence processes, while a potentially beneficial strategy for some molecular qubits, pressure slightly hardens the phonons in Na 9 [Ho(W 5 O 18 ) 2 ]·35H 2 O and systematically fills in the transparency window in the phonon response. The net result is that the vibrational spectrum becomes less sparse and the overlap with the various M J levels of the Ho 3+ ion actually increases. These findings suggest that negative pressure, achieved using chemical means or elongational strain, could further open the transparency window in this rare earth-containing spin qubit system, thus paving the way for the use of device surfaces and interface elongational/compressive strains to better manage decoherence pathways.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Near L-edge Single and Multiple Photoionization of Doubly Charged Iron Ions

Using the photon-ion merged-beams technique at a synchrotron light source, we have measured relative cross sections for single and up to five-fold photoionization of Fe 2+ ions in the energy range of 690-920 eV. This range contains thresholds and resonances associated with ionization and excitation of 2p and 2s electrons. Calculations were performed to simulate the total absorption spectra. The theoretical results show very good agreement with the experimental data, if overall energy shifts of up to 2.5 eV are applied to the calculated resonance positions and assumptions are made about the initial experimental population of the various levels of the Fe 2+ ([Ar]3d 6 ) ground configuration. Furthermore, we performed extensive calculations of the Auger cascades that result when an electron is removed from the 2p subshell of Fe 2+ . These computations lead to a better agreement with the measured product-charge-state distributions as compared to earlier work. We conclude that the L-shell absorption features of low-charged iron ions are useful for identifying gas-phase iron in the interstellar medium and for discriminating against the various forms of condensed-phase iron bound to composite interstellar dust grains.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2026

Elucidating microstructural evolution and hardness variation across friction self-piercing riveted Al-7055 using synchrotron X-ray scattering and advanced microscopy techniques

Friction self-piercing riveting (FSPR) is a unique hybrid joining technique that combines the advantages of mechanical interlocking, frictional heat, and solid-state joining (if metallurgically compatible) to produce crack free joints in high strength and/or low-ductility alloys at room temperature. Here, in the current study, Al-7055 sheets were joined using FSPR for lightweight automotive applications and significant microhardness variations were observed across the joint cross-section. A detailed microstructural characterization at multiple length scales was carried out using advanced electron microscopy and X-ray scattering techniques to provide a fundamental understanding of the process-structure-property relationships. The relative contributions of microstructural characteristics at various length scales (i.e., grain size, dislocation density, solute concentration, precipitate nature) to strengthening were estimated using existent formulations (i.e., Hall-Petch, Taylor, precipitate bypass/shear equations) and correlated to the observed microhardness values across different regions. Small-angle X-ray scattering and scanning transmission electron microscopy revealed significant changes in the size and volume fraction of precipitate species, i.e., GP-I Zones, η′, and Mg/Zn solute co-clusters, depending on the process region. It was observed that the dissolution of the small η′/GP-I zones (T ∼ 150–200 °C) in the heat-affected zone were the key reason for the hardness drop. Further, it was shown that solid-solution, dislocation, grain size and solute co-cluster strengthening played a key role in the thermo-mechanically affected zone and grain-refined zone (GRZ). Finally, these observations were leveraged along with the Zener-Holloman relationship and grain size in the GRZ to estimate the peak joining temperature of the GRZ (∼ 350 °C) near the steel rivet.

aluminum 7xxx alloy↗
NASA NTRS1997

Characterization of Cadmium-Zinc Telluride Crystals Grown by 'Contactless' PVT Using Synchrotron White Beam Topography

Crystals of Cd(1-x)Zn(x)Te grown by Physical Vapor Transport (PVT) using self-seeding 'contactless' techniques were characterized using synchrotron radiation (reflection, transmission, and Laue back-reflection X-ray topography). Crystals of low (x = 0.04) and high (up to x approx. = 0.4) ZnTe content were investigated. Twins and defects such as dislocations, precipitates, and slip bands were identified. Extensive inhomogeneous strains present in some samples were found to be generated by interaction (sticking) with the pedestal and by composition gradients in the crystals. Large (up to about 5 mm) oval strain fields were observed around some Te precipitates. Low angle grain boundaries were found only in higher ZnTe content (x greater than or equal to 0.2) samples.

Palosz, W.↗
NASA NTRS2015

Characterization of Meteorites by Focused Ion Beam Sectioning: Recent Applications to CAIs and Primitive Meteorite Matrices

Focused ion beam (FIB) sectioning has revolutionized preparation of meteorite samples for characterization by analytical transmission electron microscopy (TEM) and other techniques. Although FIB is not "non-destructive" in the purest sense, each extracted section amounts to no more than nanograms (approximately 500 cubic microns) removed intact from locations precisely controlled by SEM imaging and analysis. Physical alteration of surrounding material by ion damage, fracture or sputter contamination effects is localized to within a few micrometers around the lift-out point. This leaves adjacent material intact for coordinate geochemical analysis by SIMS, microdrill extraction/TIMS and other techniques. After lift out, FIB sections can be quantitatively analyzed by electron microprobe prior to final thinning, synchrotron x-ray techniques, and by the full range of state-of-the-art analytical field-emission scanning transmission electron microscope (FE-STEM) techniques once thinning is complete. Multiple meteorite studies supported by FIB/FE-STEM are currently underway at NASA-JSC, including coordinated analysis of refractory phase assemblages in CAIs and fine-grained matrices in carbonaceous chondrites. FIB sectioning of CAIs has uncovered epitaxial and other overgrowth relations between corundum-hibonite-spinel consistent with hibonite preceding corundum and/or spinel in non-equilibrium condensation sequences at combinations of higher gas pressures, dust-gas enrichments or significant nebular transport. For all of these cases, the ability of FIB to allow for coordination with spatially-associated isotopic data by SIMS provides immense value for constraining the formation scenarios of the particular CAI assemblage. For carbonaceous chondrites matrix material, FIB has allowed us to obtain intact continuous sections of the immediate outer surface of Murchison (CM2) after it has been experimentally ion processed to simulate solar wind space weathering. The surface amorphization and loss of OH produced by the irradiation provides important clues regarding space weathering on primitive asteroids such as the OSIRIS-Rex target 101955 Bennu.

Christoffersen, Roy↗
DOE OSTI2021

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10 −4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

3DXRD↗
DOE OSTI2023

Synthesis of Free-Standing Pd-Ni-P Metallic Glass Nanoparticles with Durable Medium-Range Ordered Structure for Enhanced Electrocatalytic Properties

Topologically disordered metallic glass nanoparticles (MGNPs) with highly active and tailorable surface chemistries have immense potential for functional uses. The synthesis of free-standing MGNPs is crucial and intensively pursued because their activity strongly depends on their exposed surfaces. Herein, a novel laser-evaporated inert-gas condensation method is designed and successfully developed for synthesizing free-standing MGNPs without substrates or capping agents, which is implemented via pulse laser-induced atomic vapor deposition under an inert helium atmosphere. In this way, the metallic atoms vaporized from the targets collide with helium atoms and then condense into short-range-order (SRO) clusters, which mutually assemble to form the MGNPs. Using this method, free-standing Pd 40 Ni 40 P 20 MGNPs with a spherical morphology are synthesized, which demonstrates satisfactory electrocatalytic activity and durability in oxygen reduction reactions. Moreover, local structure investigations using synchrotron pair distribution function techniques reveal the transformation of SRO cluster connection motifs of the MGNPs from face-sharing to edge-sharing modes during cyclic voltammetry cycles, which enhances the electrochemical stability by blocking crystallization. Further, this approach provides a general strategy for preparing free-standing MGNPs with high surface activities, which may have widespread functional applications

36 MATERIALS SCIENCE↗
DOE OSTI2022

High pressure induced atomic and mesoscale phase behaviors of one-dimensional TiO 2 anatase nanocrystals

Here, we report the high pressure phase and morphology behavior of ordered anatase titanium dioxide (TiO 2 ) nanocrystal arrays. One-dimensional TiO 2 nanorods and nanorices were synthesized and self-assembled into ordered mesostructures. Their phase and morphological transitions at both atomic scale and mesoscale under pressure were studied using in situ synchrotron wide- and small-angle x-ray scattering (WAXS and SAXS) techniques. At the atomic scale, synchrotron WAXS reveals a pressure-induced irreversible amorphization up to 35 GPa in both samples but with different onset pressures. On the mesoscale, no clear phase transformations were observed up to 20 GPa by synchrotron SAXS. Intriguingly, sintering of TiO 2 nanorods at mesoscale into nano-squares or nano-rectangles, as well as nanorices into nanowires, were observed for the first time by transmission electron microscopy. Such pressure-induced nanoparticle phase-amorphization and morphological changes provide valuable insights for design and engineering structurally stable nanomaterials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Using Complementary Methods of Synchrotron Radiation Powder Diffraction and Pair Distribution Function to Refine Crystal Structures with High Quality Parameters—A Review

Determination of the atomic-scale structures of certain fine-grained minerals using single-crystal X-ray diffraction (XRD) has been challenging because they commonly occur as submicron and nanocrystals in the geological environment. Synchrotron powder diffraction and scattering techniques are useful complementary methods for studying this type of minerals. In this review, we discussed three example studies investigated by combined methods of synchrotron radiation XRD and pair distribution function (PDF) techniques: (1) low-temperature cristobalite; (2) kaolinite; and (3) vernadite. Powder XRD is useful to determine the average structure including unit-cell parameters, fractional atomic coordinates, occupancies and isotropic atomic displacement parameters. X-ray/Neutron PDF methods are sensitive to study the local structure with anisotropic atomic displacement parameters (ADP). The results and case studies suggest that the crystal structure and high-quality ADP values can be obtained using the combined methods. The method can be useful to characterize crystals and minerals that are not suitable for single-crystal XRD.

58 GEOSCIENCES↗
DOE OSTI2024

Epitaxial oxide ionotronics: Interfaces and oxygen vacancies

Oxide ionotronics is an interdisciplinary field in which systems and devices rely on the migration of ions/ionic defects to alter or drive functionality. In this perspective, we focus on epitaxial oxide heterostructures and the contributing roles of oxygen vacancies and interfaces in ionotronics. We begin with a description of oxygen vacancy behavior, with a focus on vacancy ordering and the effects of interfaces and electric fields on particular epitaxial oxide systems. We then emphasize the use of synchrotron x-ray techniques for investigating system structure and dynamics in situ at interfaces and surfaces. Finally, an outlook on the future of epitaxial oxide ionotronics is provided, and several key areas for research are identified, such as freestanding heterostructures, combinatorial synthesis and machine learning, and next-generation synchrotron x-ray characterization.

36 MATERIALS SCIENCE↗