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Results for “High pressure X-ray diffraction”

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At least 217 records · Page 12

Side-by-side evaluation of the outgassing rate and ultimate pressure achieved inside tubes made of low-carbon and stainless steel

The hydrogen outgassing rate of a vacuum chamber made of AISI 1020 low-carbon steel was found to be notably smaller than a similar chamber made of AISI 316L stainless steel following heat treatment at 150 °C. When the chambers were baked at 400 °C, the outgassing rate of the 1020 low-carbon steel chamber was approximately 2000 times smaller than that of the 316L stainless-steel chamber. After quantifying hydrogen outgassing rates, vacuum chambers made of 1020 low-carbon steel and 316L stainless steel were heated for a prescribed duration and then pumped with an ion pump and nonevaporable getter pump to reach “ultimate pressure.” The 1020 low-carbon steel chamber reached lower pressures than the 316L stainless-steel chamber. Monte Carlo simulation predictions using the measured hydrogen outgassing rates are in good agreement with the ultimate pressure measurements. Finally, our measurements indicate that low-carbon steel can provide pressures within the extreme high vacuum range (<7.5 × 10 -13 Torr) if care is taken to minimize the surface area contribution from stainless steel.

36 MATERIALS SCIENCE↗

The CheMin XRD on the Mars Science Laboratory Rover Curiosity: Construction, Operation, and Quantitative Mineralogical Results from the Surface of Mars

The Mars Science Laboratory mission was launched from Cape Canaveral, Florida on Nov. 26, 2011 and landed in Gale crater, Mars on Aug. 6, 2012. MSL's mission is to identify and characterize ancient "habitable" environments on Mars. MSL's precision landing system placed the Curiosity rover within 2 km of the center of its 20 X 6 km landing ellipse, next to Gale's central mound, a 5,000 meter high pile of laminated sediment which may contain 1 billion years of Mars history. Curiosity carries with it a full suite of analytical instruments, including the CheMin X-ray diffractometer, the first XRD flown in space. CheMin is essentially a transmission X-ray pinhole camera. A fine-focus Co source and collimator transmits a 50μm beam through a powdered sample held between X-ray transparent plastic windows. The sample holder is shaken by a piezoelectric actuator such that the powder flows like a liquid, each grain passing in random orientation through the beam over time. Forward-diffracted and fluoresced X-ray photons from the sample are detected by an X-ray sensitive Charge Coupled Device (CCD) operated in single photon counting mode. When operated in this way, both the x,y position and the energy of each photon are detected. The resulting energy-selected Co Kalpha Debye-Scherrer pattern is used to determine the identities and amounts of minerals present via Rietveld refinement, and a histogram of all X-ray events constitutes an X-ray fluorescence analysis of the sample.The key role that definitive mineralogy plays in understanding the Martian surface is a consequence of the fact that minerals are thermodynamic phases, having known and specific ranges of temperature, pressure and composition within which they are stable. More than simple compositional analysis, definitive mineralogical analysis can provide information about pressure/temperature conditions of formation, past climate, water activity and the like. Definitive mineralogical analyses are necessary to establish the origin or provenance of a sample. The search for evidence of extant or extinct life on Mars will initially be a search for evidence of present or past conditions supportive of life (e.g., evidence of water), not for life itself.Results of the first 1,000 sols (Mars days) will be discussed, including the discovery of the first habitable environment on Mars.

CheMin↗

Postirradiation Examination of WIRE-21 Experiment Irradiated in the High Flux Isotope Reactor

Westinghouse Electric Company is developing wireless sensors to monitor the centerline temperature and internal pressure of commercial light-water reactor fuel rods during irradiation. Oak Ridge National Laboratory and Westinghouse Electric Company developed the Wireless Instrumented RB Experiment 2021 (WIRE-21) to test wireless temperature and pressure sensor technologies in a removable beryllium position in the High Flux Isotope Reactor. The experiment was irradiated for a total of 75 days, at temperatures ranging from approximately 150°C to 400°C, resulting in a peak fast (energy > 0.1 MeV) neutron fluence of about 3 × 10 21 n/cm 2 . The temperature was intentionally cycled multiple times to compare the response of the wireless temperature sensor to collocated thermocouples. Similarly, the pressure sensor was actuated in multiple steps to compare the response of the wireless measurement to excore pressure transducers (Petrie et al., 2023). After irradiation, the experiment was disassembled in the Irradiated Fuels Examination Laboratory (IFEL) hot cell at Oak Ridge National Laboratory with the intent to recover sensor and dosimetry components, document the as-irradiated condition of the hardware, and investigate possible causes of the sensor behavior observed during irradiation. The postirradiation examination successfully recovered and preserved key WIRE-21 components. After the housing was removed using a milling machine, the internal experiment sections were examined. All eight fiber-optic sensors were recovered, cut, and stored. The silicon carbide thermometry, temperature sensor, pressure sensor, lower spacer, and selected pressure and temperature cable sections were also removed and stored. The metal bellows of the pressure sensor was found to be plastically deformed, indicating that it had been properly pressurized during irradiation and generally behaved as expected. X-ray diffraction analysis of a section of one of the irradiated inductor cores within the pressure sensor was performed and confirmed the presence of phase-pure alpha ferrite (i.e., no unexpected phase transformations). Inductance testing was performed on the irradiated pressure sensor cores using an unirradiated test coil, and DC resistance measurements of the transceiver coils were also performed. The measurements with irradiated inductor cores assembled inside unirradiated coils showed slightly reduced inductance compared to measurements made with unirradiated cores, but the difference was not sufficient to explain the more significant reductions in inductance that were observed in-pile. Therefore, it is suspected that degradation of the inductor coils (specifically the wire wrapping) is responsible for the reduced inductance observed in-pile.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Exploring the Geochemistry of Tholeiitic Basalts and Hyaloclastites Formed in Submarine Volcanoes for Comparison With Venus Lavas

Underwater basaltic lavas exhibit distinct rock textures, mineralogy and morphological differences compared to those formed on land, primarily due to rapid cooling caused by contact with cold seawater instead of air and to high pressures – similar to Venus. The geomorphological similarities between terrestrial submarine volcanoes and some morphological classes of Venusian volcanoes have been investigated, but a comprehensive comparison in geochemical terms has yet to be conducted. Only three missions to Venus (Venera-13, Venera-14, and Vega-2) were able to report bulk composition of Venusian rocks, while other four missions (Venera-8, Venera-9, Venera-10, and Vega-1) provided limited geochemical information. Using X-Ray fluorescent (XRF) analysis, we saw that rocks analyzed on the surface of Venus are tholeiitic and alkalic basalts. This study, as part of the “Analogs for VENus's GEologically Recent Surfaces” (AVENGERS) initiative, aims to examine the possibility of seamounts/submarine volcanoes lavas serving as analogues to Venus lava geochemistry and morphology/formational processes. By sampling and analyzing submarine lavas from three distinct tectonic settings on Earth - hot-spot, convergent margins, and divergent margins - we will assess in which tectonic context the analogy with Venus is most comparable. Fieldwork will be conducted in further detail for submarine volcanoes located in Sicily, Hawaiʻi, and the Southern Pacific (Fiji, Vanuatu, Tonga, Samoa); we will use previously collected samples where these submarine areas are not accessible. Sampling efforts will target areas likely to yield submarine tholeiitic lavas and/or hyaloclastites. Samples collected during fieldwork will undergo detailed whole-rock geochemical analysis, including XRF, X-Ray diffraction (XRD) and Inductively Coupled Plasma Mass Spectrometry (ICPMS). Thin sections will be used to constrain differences in morphology/textures. The obtained geochemical data will then be compared with existing data on Venusian lava geochemistry, allowing for a comprehensive evaluation of potential analogies between submarine lavas from Earth and volcanic rocks on Venus. By elucidating these similarities and pinpointing specific tectonic contexts, our study has the potential to enhance our understanding of Venusian geology and the possibility of ephemeral plate tectonics on the planet.

N Mari↗

Pressure-Induced Chemical Bonding Effects on Lattice and Magnetic Instabilities in Antiferromagnetic Insulating CaMn 2 Sb 2

Exotic quantum phenomena often emerge near an electronic delocalization transition (EDT) from an antiferromagnetic insulating phase to a strongly correlated metallic state under pressure. We report the pressure-induced structural and magnetic evolution of the antiferromagnetic insulator CaMn 2 Sb 2 . Single-crystal X-ray diffraction reveals a first-order phase transition near 5.4 GPa from a trigonal P-3m1 structure to a monoclinic P2 1 /m phase accompanied by a ∼7% volume collapse. Residual electron density analysis at intermediate pressures reveals charge localization along Mn–Sb chains, signaling electronic instability preceding the structural transition. Bonding analysis indicates anisotropic Mn–Sb orbital reconfiguration under pressure, driving a distorted square-pyramidal geometry. Neutron scattering confirms the transition and identifies a pressure-induced incommensurate magnetic order, distinct from the ambient antiferromagnetic state. In the monoclinic phase, zigzag Mn chains exhibit antiferromagnetic coupling along the ac-plane, enabled by enhanced orbital overlap. These results establish CaMn 2 Sb 2 as a model system for studying the coupling of structural distortion, charge redistribution, and magnetic order in layered Mn pnictides under pressure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Machine Learning Approaches for Rare-Earth Silicate Environmental Barrier Coating Thermochemical and Thermomechanical Property Predictions

Environmental barrier coatings (EBCs) are a necessary enabling technology for the transition from superalloys to silicon carbide (SiC) ceramic matrix composites (CMCs) in gas turbine engines for increased efficiency and decreased fuel costs. SiC-based CMCs are prone to oxidation-based degradation in the engine hot section, and rare-earth (RE) silicates are promising candidates for EBCs due to their close thermal expansion match to the composite substrate and oxidation resistance. However, the design of EBCs is hindered by the large chemical space of candidate materials and the difficulty in obtaining material properties for engineering optimization. This is especially difficult as research continues into mixed-cation or “high-entropy” RE silicates. First-principles computational methods such as density functional theory (DFT) are highly effective at calculating material properties to guide coating design but are limited by their computational cost. Atomistic simulations have the potential to both accelerate property calculations and expand the properties able to be calculated due to their lower computational compared to DFT. However, they require interatomic potentials (IAPs) specific to the material system of interest, and, to our knowledge, there are no suitable IAPs for RE silicates. Machine learning (ML) is a promising technique to accelerate material property predictions indirectly by generating IAPs for atomistic simulations or via direct prediction. In this work, we present two ML approaches to accelerate the calculation of RE silicate properties relevant to EBC design: 1) a ML-derived interatomic potential (IAP) for atomistic simulations of yttrium disilicate (Y2Si2O7) from DFT training data, and 2) a neural network (NN) model to directly predict thermochemical properties of RE silicates and oxides directly from easily obtainable unit cell parameters. Classical MD simulations using the IAP yield lattice properties and bond lengths in good agreement with both DFT and experimental results from x-ray diffraction. Thermodynamic properties calculated using the finite-displacement phonon method and quasi-harmonic approximation were orders of magnitude faster than DFT with good agreement to the DFT results. The IAP was also used to calculate properties such as coefficient of thermal expansion (CTE) that require large simulation supercells and are therefore difficult with DFT. The IAP correctly predicted the anisotropic nature of the CTE in three different phases of Y2Si2O7. The NN model predicts constant pressure heat capacity, Cp, orders of magnitude faster than DFT calculations, which can enable its use as a surrogate model for multiscale simulations. The two methods presented in this work demonstrate the utility of ML for accelerating the prediction of RE silicate properties, which can in turn accelerate EBC design and optimization.

machine learning↗

Experimental Studies on the Effect of Impact Processes on the Formation and Evolution of Amino Acids

Introduction: A critical step in the emergence of life on Earth was the synthesis of larger organic molecules from simple building blocks such as NH3, CO2, H2O, and CH3OH. The presence of amino acids and other complex organics in comets and meteorites demonstrates that widespread organic synthesis likely occurred across the early solar system. Building on previous work [e.g., 1-3], we systematically explore impact-driven chemical evolution of exogenous organics and their precursors. Collisional processes may also have provided a source of energy for the formation of more complex organics from endogenous building blocks. The high flux of impactors to Earth immediately prior to and during the origins of life suggests that impacts could have played a critical role. Key Questions: 1. How are the formation and evolution of amino acids affected by the presence of a mineral matrix during cometary and asteroidal impacts onto the early Earth? 2. Do some minerals (e.g., phyllosilicates) provide a more robust protective framework or reactive surface site for amino-acid formation and/or polymerization? 3. Does the abundance of ices and/or amino acids relative to that of the mineral matrix affect the formation and evolution of amino acids? 4. Are there impact velocities/shock pressures at which formation or polymerization of amino acids is favored or precluded? Experimental Approach: This study systematically examines the conditions under which amino acids and other organic molecules can form, be polymerized, and/or be destroyed during impact events into particulate regolith simulants. Variable parameters include the modal composition of this regolith (silicate matrices, ratios of ices, silicates, and amino acids) and impact velocities/shock pressures. Impacts experiments were performed using the two-stage light-gas gun (LGG), vertical gun (VG), and flat-plate accelerator (FPA) in the Experimental Impact Lab at JSC. FPA experiments were performed over a range of shock pressures (11.3-31.5 GPa) using CM chondrite simulant mixed with amino acids at ratios of 0:10, 1:10, 1:103, and 1:106 (amino acid:host). Techniques for mixing cometary ices have been optimized and test runs have been performed using the LGG (see figure below). Analysis: Post-impact, samples are heated in water to extract amino acids and peptides. Extracts are characterized via liquid chromatography-mass spectrometry (LC-MS) and the mineralogies of solid residues are characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Additional LC-MS and mineralogical analyses are underway.

Eve L Berger↗

Ammonolysis with N 2 -diluted NH 3 suppresses Ta( IV ) defects in BaTaO 2 N and enhances photocatalytic water oxidation

BaTaO 2 N stands out among oxynitride photocatalysts because of its ability to capture visible light and to drive the photoelectrochemical water oxidation reaction. However, its solar energy conversion performance is limited by electron–hole recombination at Ta( IV ) defects in the material. These defects are formed by overreduction of the Ta(v) oxide precursor by excess ammonia under the high temperature conditions during ammonolysis. Here we show for the first time that Ta( IV ) defect concentrations can be lowered by conducting the ammonolysis reaction in mixed NH 3 /N 2 gas. The obtained BaTaO 2 N samples crystallize in the cubic CaTiO 3 structure type and form 200–300 nm faceted nanocrystals, based on X-ray diffraction, scanning electron microscopy, and HRTEM. Electron paramagnetic resonance spectra observe the Ta( IV ) defects at g = 1.999 and confirm an 11-fold reduction for the product synthesized in mixed (0.13 : 1.0 vol) NH 3 /N 2 gas, equivalent to 1.14 × 10 16 cm −3 Ta( IV ) ions. This optimized BaTaO 2 N has nearly twice the photocatalytic oxygen evolution activity (AQE of 6.78% at 400 nm) of a reference material made with 1.0 atm ammonia and 78% higher photoelectrochemical water oxidation photocurrent (0.9 mA cm −2 at 1.23 V vs. RHE) under simulated sunlight. According to X-ray photoelectron spectroscopy, remaining Ta( IV ) defects are concentrated in the surface region of the BaTaO 2 N particles, where >50% of all Ta ions are found in the +4 oxidation state. This surface Ta( IV ) population can be directly observed in Vibrating Kelvin Probe Surface Photovoltage Spectra (VK-SPV) via its 1.2–1.4 eV photovoltage onset. Here, it suggests that the surface Ta( IV ) ions contribute empty d-states 0.5–0.7 eV below the BaTaO 2 N conduction band edge. These findings highlight how the energetics and concentrations of Ta( IV ) defects influence the photoelectrochemical water oxidation ability of BaTaO 2 N. Additionally, the work establishes ammonolysis with diluted NH 3 as a new tool to minimize defects in BaTaO 2 N and to raise its solar energy conversion efficiency toward its theoretical limit. Because of its simplicity, the reduced ammonia pressure strategy will likely be applicable to other oxynitrides, which generally suffer from overreduction problems during ammonolysis.

Salmanion, Mahya [University of California, Davis,↗

Influence of Compositional Complexity on Amorphization Resistance of Swift Heavy Ion Irradiated Titanate Pyrochlores

Compositionally complex oxides have garnered attention recently for their potential technological applications in harsh environments such as thermal barrier coatings and nuclear waste forms. Therefore, their response to extreme conditions, including high temperature and intense irradiation fields, must be thoroughly investigated. Here, the structural evolution of two pyrochlore oxides with comparable cation size ratio, r A /r B , (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 and Ho 2 Ti 2 O 7 , was evaluated after irradiation with 946 MeV Au ions up to a fluence of 8 × 10 12 ions/cm2 using synchrotron X-ray diffraction, transmission electron microscopy, and Raman spectroscopy. The overall radiation response is comparable for both titanate oxides and is dominated by a loss of crystallinity. When compared to a series of conventional titanate pyrochlore compositions, the amorphous track diameter of (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 is slightly larger than that of Ho2Ti2O7 and more in line with the diameter of the endmember with the maximum A-site cation size (Gd 2 Ti 2 O 7 ). Density functional theory calculations suggest that this behavior may be linked to local lattice distortions and the associated energetics of cation antisite formation. TEM and Raman analyses show that a disordered, crystalline shell surrounds the amorphous ion tracks in (Yb 0.2 Er 0.2 Dy 0.2 Tb 0.2 Gd 0.2 ) 2 Ti 2 O 7 , and the corresponding short-range structure resembles a weberite-type atomic arrangement.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diagnostic Clast-Texture Criteria for Recognition of Impact Deposits

It is difficult to find definitive evidence for impact in the geological record because there are many endogenous geological processes that can produce diamictites similar to those generated by impact ejecta. The classic impact criteria of shock fabrics in certain minerals, and iridium layers, for example, may be either difficult to find, or long-since erased from the impact site (shock fabrics also anneal with time). It is important to be able to recognize impact-generated materials in order to understand earth's crustal development and biological evolution. In future exploration of Mars and other solar-system bodies, recognition of impact materials will be important for elucidating planetary evolution, planetary volatile inventories, and exobiological issues. The cobble depicted is typical of many that have been found in diamictite deposits in Belize generated by the Chicxulub K-T impact event. The pebbles are roughly-hewn in general shape with smoothed corners and edges. Surfaces are almost uniformly frosted (on both protuberances and hollows), but some asperities are glazed. Optical microscopy and thin-section petrographic microscopy reveal the frosting to be only a few microns thick, with a well-defined granular structure; grains are the same size as those composing the bulk of the limestone, but their clearer appearance may represent annealing. One or two adjacent pebble faces are often decorated with striated gouges and closely-spaced hemispherical depressions representing indentation hollows produced by well-rounded impacting clasts of up to 0.5 cm in diameter. Some of the impactors are still embedded in the cobble surface. Non-destructive x-ray diffraction techniques showed the impactors to be of the same mineralogy as the target cobble. We believe this unusual glazing and frosting to be related to the impact event, but this must be reconciled with its survival for over 60 my. since it is composed of one of the most alterable substances, CaCO3. We focus, however, on the non-fractured rounded pebbles that appear to have impacted the larger cobble as a swarm of clasts, probably encountered during ballistic flight. It cannot be defined whether the cobble swept through the pebble cloud, or the pebbles rained upon a slowermoving cobble. Two interesting questions arise: (1) Where did large numbers of such well rounded pebbles come from in the ejecta curtain?, and (2) How did they embed themselves in a nominally brittle rock without suffering damage? Are the well-rounded pebbles crystalline (devitrified) melt spherules? Further investigations are in progress. If the cobble was cold and brittle, impact of well-rounded pebbles would have produced Hertzian fracture patterns (a) in the virtually elastically isotropic cobble target. For penetration depths of about 0.5 of the impactor diameter, the pebbles would require a relative impact velocity sufficient to cause pebble fragmentation and crushing, and the development of a complex Hertzian-Boussinesq fracture field (b) involving deep fracturing and lateral surface spalling (impact velocities > 50 m/s). The existing relationship could only evolve by the impact of cold, hard pebbles into a soft, plastic cobble surface (c). For limestone to have been plastic, it must have been at elevated temperature, but to prevent calcification of the material, the ambient pressure must also have been elevated. This would be possible either in the impact's gas plume, or within the confines of a thin aerodynamically-produced shock bow generated by supersonic ballistic motion of the cobble. In the latter case, it is implied that the cobble swept through the pebbles rather than vice-versa. Although there are high T-P conditions associated with volcanism, such textures have not been reported on volcaniclastic materials, nor from other high T-P environments; e.g., metamorphic (as far as the authors are aware). We propose that this very easily recognizable embedding and indentation surface texture can be used as a diagnostic criterion for the recognition of impact ejecta. The term "peening texture" is suggested, because it is absolutely analogous to the plastic-deformation induced, metal-surface textures generated by ball-bearing bombardment used in engineering metallurgy to work-harden metal surfaces. Additional information is contained in the original (Figures).

Marshall, J. R.↗

Shock compression of crystalline TeO 2 to the high-pressure fluid regime: Insights from ab initio molecular dynamics simulations

The shock response of fully-dense and porous crystalline tellurium dioxide (TeO 2 ⁠) to the high-pressure and high-temperature fluid regime was investigated within the framework of density functional theory with Mermin’s generalization to finite temperatures. The principal and porous shock Hugoniot curves were predicted from canonical ab initio molecular dynamics (AIMD) simulations, with the phase space sampled along isotherms up to 80 000 K, for densities ranging from ρ = 3 to 17 g/cm 3 . The polymorphs investigated are α-TeO 2 paratellurite (⁠P4 1 2 1 2), TeO 2 cotunnite (⁠Pnma⁠), and TeO 2 post-cotunnite (⁠P2 1 /m⁠). Based on the discontinuity found in the calculated U s – u p slope of TeO 2 post-cotunnite at a shock velocity of U s ≃ 8.35km/s and a particle velocity of u p ≃ 3.64 km/s, the shock melting temperature and pressure are predicted to be ≃ 6500 K and ≃ 170 GPa. Results from the AIMD simulations are in line with the static compression data of TeO 2 paratellurite and cotunnite, and with the recent shock Hugoniot data for single-crystal α- TeO 2 for pressures up to 85 GPa, obtained using the inclined-mirror method and the velocity interferometer system for any reflector combined with powder gun and two-stage light-gas gun.

74 ATOMIC AND MOLECULAR PHYSICS↗

Thermodynamic origin of the pressure-induced Invar effect: General criterion and experimental study of Fe 68 ⁢Pd 32

Synchrotron X-ray diffraction measurements were performed on 57 Fe 68 Pd 32 at multiple pressures and two temperatures in a diamond-anvil cell. Between 4 and 11GPa, the thermal expansion was zero or slightly negative. This pressure-induced Invar effect was studied further with 57 Fe nuclear forward scattering and nuclear resonant inelastic X-ray scattering to obtain information on the pressure-induced changes in both the magnetization and the phonon density of states. Magnetic entropy and phonon entropy were obtained from these results, the latter with additional measurements from inelastic neutron scattering to account for the contributions from Pd atoms. The dependencies of these entropies on pressure gave the magnetic and phonon contributions to thermal expansion. These canceled in the region of pressure-induced Invar behavior, even though they individually increased by more than a factor of 2 below the Curie pressure. The behavior of phonons gives evidence for spin-phonon interactions in Fe 68 Pd 32 . A general explanation of the pressure-induced Invar effect is presented, showing that Invar behavior is typically expected at a pressure P* below a magnetic transition at pressure PC. The difference in pressure P C − P* scales with the fractional reduction in magnetic exchange interaction divided by the average Gr¨uneisen parameter.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Effect of pressure cycling and compression rate on the bcc-hcp transition in an FeNi alloy

Here, we investigate the body-centered cubic (bcc) to hexagonal close-packed (hcp) phase transition in Fe-10wt. %Ni alloy, combining pressure cycling and fast compression with time-resolved synchrotron x-ray diffraction in a dynamic diamond anvil cell. Three pressure cycles were conducted with compression rates ranging from 0.1 to nearly 10 3 GPa/s. During the first cycle with the slowest compression, the observed orientations in the bcc and hcp phases are consistent with the Burgers mechanism, followed by c-axis rotation of the hcp phase consistent with {$10$ $\bar{1}2$} twinning. During the following cycles with fast compression at 10 2 –10 3 GPa/s, the hcp phase exhibits negligible c-axis rotation with a nearly constant c/a ratio of ∼1.61 up to ∼30 GPa, indicating suppression of plastic deformation (especially, twinning) due to sample confinement from the gasket. Notably, the onset pressure of the transition decreases with additional pressure cycling and faster compression, which normally leads to over-pressurization. This suggests that defects or shear induced from the pressure cycling reduces the transition kinetics even during fast compression. These insights into the deformation and transition behavior in an FeNi alloy under multiple dynamic loading cycles can offer guidance for future design of advanced structural alloys and improve our understanding of planetary core processes.

FeNi alloy↗

Mineralogical Analysis of Calcium-Aluminum-Rich Inclusions Provides Insight Into Post-Formation Processes

Introduction: Calcium-aluminum inclusions (CAIs) are cm- to mm-sized intergrowths of refractory phases found in chondritic meteorites [1]. Their mineral compositions closely match the compositions of the solids thought to condense from an extremely hot (>1500K) gas with a bulk solar composition [2-4], suggesting that CAIs were the earliest solids within the Solar System [2-4]. These inclusions provide invaluable insights into the conditions and dynamics of the early Solar System. CAIs must be transported from their formation region near the protosun to the chondrite parent-body accretion region. The nature of their journey could affect how, when, and where the secondary processes recorded in these CAIs occurred [4]. Did these secondary processes occur in the solar nebula or during accretion with the parent body, or both? How were the CAIs affected by varying thermochemical processes? To better answer these questions, we have undertaken an in-depth, textural study of the secondary alteration of select CAI samples. Methods: We chose three CAIs that experienced a range of post-formation processing to gain better understanding of secondary alteration based on previous preliminary examination [5]. Representative CAIs were chosen from NWA 5508 (CV3), NWA 12772 (CV3), and Coolidge (CL4) carbonaceous chondrites. We used scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) techniques for detailed chemical, mineralogical, and textural analysis of the CAIs. Backscattered electron (BSE) images and X-ray elemental maps were taken of Coolidge and NWA 5508 using the Lunar and Planetary Institute (LPI) Phenom SEM. The JEOL 7900F SEM at NASA Johnson Space Center (JSC) was used to obtain energy dispersive spectroscopy (EDS) chemical maps of all samples. High resolution EBSD analysis identified the mineral phases and textures, providing key information on their nature. Based on the SEM and EBSD data, minerals of interest were selected for quantitative chemical electron probe micro-analysis (EPMA) using the JEOL JXA-8530F at NASA JSC. Results and Discussion: The EDS maps show that the NWA 5508 and NWA 12772 CAIs designated “Saguaro” and “Hoopoe” respectively [5] are enriched in calcium while the Coolidge CAI designated “Cottonwood” is aluminum and magnesium rich. Saguaro. A ~1.5cm diameter igneous Type B CAI with a rounded shape. The dominant phases are melilite, spinel, and Al-Ti pyroxene with minor anorthite. Spinel is subhedral and occurs in clusters. Some of these clusters have a circular geometry which encloses other minerals, known as a palisade structure [6] (Fig. 1). Some palisades form near perfect circles while others are more irregular in shape. Melilite in Saguaro ranges in size from coarse (>250m) to fine-grained (5-7m) and forms intergrown laths. A third of the melilite grains exhibit simple twinning about their <001> axis. The spinel palisades and twinned melilite in Saguaro suggest an igneous history, and the lack of secondary minerals suggests minimal aqueous alteration. At some point in time after the initial condensation of the minerals and formation of the inclusion, the sample was remelted and quickly solidified. The formation of the palisades is still heavily debated. One hypothesis is that the palisades are the rims of smaller CAIs that accreted early on, essentially acting as xenoliths within the larger CAIs [7]. Another hypothesis suggests an igneous origin for palisade structures [6-8] wherein the melt traps gas bubbles, and the spinel nucleates on the surface of this bubble. Based on the WDS spot analyses of 41 melilite grains using EPMA, the data suggest that the composition inside and outside the palisades is nearly identical. This finding indicates that these palisades are likely not exogenous but rather formed from melt-vapor reactions. Our results are consistent with studies by Simon and Grossman,1997 [6] and Zhang et al. (2019) [8]. Hoopoe. A ~0.5cm compact Type A CAI with an irregular shape. The dominant mineral phases are melilite, spinel, and hibonite with minor amounts of anorthite, augite, and perovskite. The melilite ranges in size from ~500 to 50µm. The larger melilite grains have simple twinning along the <001> axis like melilite in Saguaro. Melilite in Hoopoe exhibits crystal-plastic strain with misorientation dominantly about the <010> and <110> axes. Spinel shows subhedral to euhedral morphology and appears in clusters. Hibonite grains are similar to spinel in habit and size but show more plastic strain. The two minerals are often found together with one appearing to replace the other. Perovskite appears in fine grained recrystallized regions alongside fine augite and spinel. The abundant strain and deformation features in the melilite and hibonite suggest that Hoopoe experienced shock. This shock could have occurred in the nebula [9] or from an impact of another body on the parent body asteroid. The appearance of fine-grained (<10m) areas of augite, perovskite, and spinel in the dominantly coarse-grained inclusion suggest recrystallization, possibly due to the sudden increase in pressure and temperature. Cottonwood. This ~0.5cm CAI exhibits distinct mineralogy and textures suggesting a high degree of alteration. It is irregular in shape. The dominant mineral phases are spinel and anorthite with minor amounts of augite and rutile. The two main texture types can be seen in Fig. 2. The first type consists of coarse euhedral to subhedral spinel and anorthite. The second includes fine grained spinel, anorthite, rutile, and iron sulfides. Within these fine-grained regions, the anorthite grains are clustered into domains exhibiting the same crystallographic orientation. Rutile exclusively occurs with fine anorthite indicating a potential relationship between the two. Cottonwood has a clear and unbroken Wark-Lovering [10] rim (Fig. 2) on one side that consists of a sequence of spinel followed by anorthite and an outer layer of augite. The abundance of the fine-grained regions containing iron oxides and iron sulfides, secondary phases such as rutile, and oriented anorthite grains is evidence for recrystallization associated with a high degree of thermal metamorphism. The EPMA analyses on both coarse- and fine-grained spinel show that the fine spinel grains are more enriched in Cr (1-2 wt. %) than their coarse counterparts (0.1-0.5 wt. %). The data suggest thermal metamorphism drove chemical exchange of the previously refractory inclusion, introducing chromium and iron as well as sulfur, which is moderately volatile. Conclusions: The three CAIs analyzed record distinct secondary nebular and parent body processes. Saguaro melted in the nebula as seen by the twinned melilite and spinel palisades. Hoopoe experienced intense shock which deformed its melilite and recrystallized perovskite, augite, and spinel in fine-grained regions. Cottonwood shows evidence of recrystallization and chemical changes consistent with thermal metamorphism occurring after accretion into the parent-body.

V E Burnette↗

Femtosecond temperature measurements of laser-shocked copper deduced from the intensity of the x-ray thermal diffuse scattering

We present 50-fs, single-shot measurements of the x-ray thermal diffuse scattering (TDS) from copper foils that have been shocked via nanosecond laser ablation up to pressures above ∼135 GPa. We hence deduce the x-ray Debye–Waller factor, providing a temperature measurement. The targets were laser-shocked with the DiPOLE 100-X laser at the High Energy Density endstation of the European X-ray Free-Electron Laser. Single x-ray pulses, with a photon energy of 18 keV, were scattered from the samples and recorded on Varex detectors. Despite the targets being highly textured (as evinced by large variations in the elastic scattering) and with such texture changing upon compression, the absolute intensity of the azimuthally averaged inelastic TDS between the Bragg peaks is largely insensitive to these changes, and allowing for both Compton scattering and the low-level scattering from a sacrificial ablator layer provides a reliable measurement of $T/Θ^2_D$, where Θ D is the Debye temperature. We compare our results with the predictions of the SESAME 3336 and LEOS 290 equations of state for copper and find good agreement within experimental errors. We, thus, demonstrate that single-shot temperature measurements of dynamically compressed materials can be made via thermal diffuse scattering of XFEL radiation.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Calibration and characterization of the line-VISAR diagnostic at the HED-HIBEF instrument at the European XFEL

In dynamic-compression experiments, the line-imaging Velocity Interferometer System for Any Reflector (VISAR) is a well-established diagnostic used to probe the velocity history, including wave profiles derived from dynamically compressed interfaces and wavefronts, depending on material optical properties. Knowledge of the velocity history allows for the determination of the pressure achieved during compression. Such a VISAR analysis is often based on Fourier transform techniques and assumes that the recorded interferograms are free from image distortions. In this paper, we describe the VISAR diagnostic installed at the HED-HIBEF instrument located at the European XFEL along with its calibration and characterization. It comprises a two-color (532, 1064 nm), three-arm (with three velocity sensitivities) line imaging system. We provide a procedure to correct VISAR images for geometric distortions and evaluate the performance of the system using Fourier analysis. We finally discuss the spatial and temporal calibrations of the diagnostic. As an example, we compare the pressure extracted from the VISAR analysis of shock-compressed polyimide and silicon.

47 OTHER INSTRUMENTATION↗

High pressure cosmochemistry of major planetary interiors: Laboratory studies of the water-rich region of the system ammonia-water

Several studies relative to high pressure cosmochemistry of major planetary interiors are summarized. The behavior of gas-ice mixtures at very high pressures, studies of the phase diagram of (NH3) sub x (H2O) sub 1-x at pressures to 5GPa and temperatures from 240 to 370 K, single crystal growth of ammonia dihydrate at room temperature in order to determine their structures by x-ray diffraction, spectroscopy of chemical reactions during shock compression in order to evaluate how the reactions affect the interpretation of equation of state data obtained by shock methods, and temperature and x-ray diffraction measurements made on resistively heated wire in diamond anvil cells in order to obtain phase and structural data relevant to the interiors of terrestrial planets are among the studies discussed.

Nicol, Malcolm↗

High rate reactive sputtering of MoN(x) coatings

High rate reactive sputtering of MoN(x) films was performed using feedback control of the nitorgen partial pressure. Coatings were made at four different target powers: 2.5, 5.0, 7.5 and 10 kW. No hysteresis was observed in the nitrogen partial pressure vs. flow plot, as is typically seen for the Ti-N system. Four phases were determined by X-ray diffraction: molybdenum, Mo-N solid solution, Beta-Mo2N and gamma-Mo2N. The hardness of the coatings depended upon composition, substrate bias, and target power. The phases present in the hardest films differed depending upon deposition parameters. For example, the Beta-Mo2N phase was hardest (load 25 gf) at 5.0 kW with a value of 3200 kgf/sq mm, whereas the hardest coatings at 10 kW were the gamma-Mo2N phase (3000 kgf/sq mm). The deposition rate generally decreased with increasing nitrogen partial pressure, but there was a range of partial pressures where the rate was relatively constant. At a target power of 5.0 kW, for example, the deposition rates were 3300 A/min for a N2 partial pressure of 0.05 - 1.0 mTorr.

Rudnik, Paul J.↗