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Results for “High pressure X-ray diffraction”

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NASA NTRS2003

New Directions in Biotechnology

The macromolecule crystallization program within NASA is undergoing considerable pressure, particularly budgetary pressure. While it has shown some successes, they have not lived up to the expectations of others, and technological advances may rapidly overtake the natural advantages offered by crystallization in microgravity. Concomitant with the microgravity effort has been a research program to study the macromolecule crystallization process. It was believed that a better understanding of the process would lead to growth of improved crystals for X-ray diffraction studies. The results of the various research efforts have been impressive in improving our understanding of macromolecule crystallization, but have not led to any improved structures. Macromolecule crystallization for structure determination is "one of", the job being unique for every protein and finished once a structure is obtained. However, the knowledge gained is not lost, but instead lays the foundation for developments in new areas of biotechnology and nanotechnology. In this it is highly analogous to studies into small molecule crystallization, the results of which have led to our present day microelectronics-based society. We are conducting preliminary experiments into areas such as designed macromolecule crystals, macromolecule-inorganic hybrid structures, and macromolecule-based nanotechnology. In addition, our protein crystallization studies are now being directed more towards industrial and new approaches to membrane protein crystallization.

Source record↗

DOE OSTI2026

Growth-controlled twinning and magnetic anisotropy in CeSb 2

Cerium diantimonide (CeSb 2 ) is a layered heavy-fermion Kondo lattice material that hosts complex magnetism and pressure-induced superconductivity. The interpretation of its in-plane anisotropy has remained unsettled due to structural twinning, which superimposes orthogonal magnetic responses. Here, in this study, we combine controlled crystal growth with magnetization and rotational magnetometry to disentangle the effects of twinning. Nearly untwinned high-quality single crystals reveal the intrinsic in-plane anisotropy: The in-plane easy axis saturates at 𝑀 easy ⁡(4 T) ≈ 1.8 𝜇 B /Ce, while the in-plane hard axis magnetization is strongly suppressed, nearly linear, and comparable to the out-of-plane response. These results resolve long-standing discrepancies in reported magnetic measurements, in which in-plane metamagnetic transition fields and saturation magnetization varied significantly across previous studies. Growth experiments demonstrate that avoiding the proposed 𝛼 𝛽 structural transition—through Sb-rich flux and slower cooling—systematically reduces twinning. However, powder x-ray diffraction and differential thermal analysis measurements show no clear evidence of a distinct 𝛽 phase. Our results establish a consistent magnetic phase diagram and provide essential constraints for crystal-electric field models, enabling a clearer understanding of the interplay between anisotropic magnetism and unconventional superconductivity in CeSb 2 .

Weber, Jan T. [Goethe University, Frankfurt (Germa↗

DOE OSTI2025

Continuous Evolution of Eu 2+ /Eu 3+ Mixed Valency Driven by Pressure and Temperature

Continuous mixed valency involving Eu 2+ and Eu 3+ in Eu 4 Bi 6 Se 13 can be induced under applied pressure or at reduced temperatures. The monoclinic structure of Eu 4 Bi 6 Se 13 , crystallizing in the P2 1 /m space group (No. 11), features linear chains of Eu atoms aligned along the b-axis. Magnetic susceptibility measurements, conducted both parallel and perpendicular to the b-axis and analyzed using Curie–Weiss theory, alongside high-pressure partial fluorescence yield (PFY) data from X-ray absorption spectroscopy (XAS), indicate the material’s propensity to adopt a mixed-valent state. Within this state, the trivalent Eu 3+ configuration becomes increasingly favored as the pressure rises or the temperature decreases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1995

An investigation of the loss of ductility in hydrogen charged beta-Ti alloys

The high strength, low density, and good corrosion resistance of Ti-based alloys make them candidate materials for a number of applications in the aerospace industry. A major limitation in the use of these alloys in the advanced hypersonic flight vehicle program is their susceptibility to hydrogen embrittlement. This study focuses on the hydrogen sensitivity of TIMETAL 21S beta-Ti alloy. The material received was in the form of grip-ends of failed tensile test samples which had been exposed to different charging conditions (combinations of hydrogen pressure and temperature). The samples received, the charging conditions, and their fracture mode are discussed. It can be seen that the fracture behavior changes from ductile to brittle with increasing hydrogen content, but the transition in behavior occurs for a small increase in hydrogen concentration. The aim of this program was to assess the microstructural differences between the ductile and brittle alloys to ascertain the embrittlement mechanism. A range of tools which included x-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used.

Robertson, Ian M.↗

DOE OSTI2025

Cold-Sprayed NMC622 Composite as a Cathode for Lithium-Ion Batteries

The growing demand for high-energy, low-cost lithium-ion batteries (LIBs) to power electric vehicles (EVs) necessitates advances in both materials and manufacturing processes. Conventional cathode fabrication methods, such as slurry casting and drying, are energy-intensive and pose challenges for scalability and environmental compliance. In this study, we propose cold-spray (CS) deposition as a solvent-free approach for fabricating LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) composite cathodes. Powder blends of NMC622, poly(vinylidene fluoride) (PVDF), and carbon black (CB) are directly deposited onto stainless steel and Inconel substrates under varied gas temperatures, pressures (and thus velocities), and standoff distances. The effects of temperature on the deposit morphology, coating density, and volume are systematically investigated. Computational fluid dynamics simulations reveal that increasing the gas temperature enhances the particle velocity, narrows the spray angle, and reduces the mass concentration radially at the nozzle outlet. CS deposition results in a dense cathode microstructure, accompanied by fracture in polycrystalline NMC622 particles. X-ray diffraction analysis further verifies that there are no phase changes during the deposition process. The electrochemical performance of the cold-sprayed cathodes reveals an initial capacity of approximately 96 mAh g –1 for single-crystal NMC622 and 167 mAh g –1 for polycrystalline NMC622. While these values are modest compared to state-of-the-art slurry-cast cathodes, which typically exhibit 180–200 mAh g –1 under optimized conditions. The results demonstrate a competitive performance given the solvent-free nature of the CS process and compare favorably with tape-cast samples made from identical feedstock. In conclusion, he CS process enables the formation of dense, binder-integrated cathode coatings without the need for solvent processing, offering a promising pathway for scalable, energy-efficient dry electrode manufacturing of next-generation LIBs.

Batteries↗

NASA NTRS2001

High-Pressure Synthesis of Metal-Ceramic Nano-Composites

The major problems in fabrication of nano-crystal line materials form nano-powders are: (1), coarsening of the initial nano-size grains, (2), insufficient densification (high concentration of pores), and, (3), conversion of diamond into graphite (for diamond-based ceramics). We have developed a novel technique of the synthesis of nano-composite materials applying very high (up to about 10 GPa) pressures. In this technique, one component is pre-compacted and placed next to another having a lower melting point temperature. The whole sample is pressed and the temperature raised above the melting point of the second component, what results in the melt getting pressed into the (nano-size) pores of the compact. Upon subsequent crystallization the melt forms the second nanophase. The process is fast, on the order of seconds, and the temperatures are relatively low what prevents, or at least significantly reduces coarsening of the starting nanophase grains. Also, conversion of diamond into graphite can be prevented. The technique allows for control of the final product properties through a proper selection of (1) the initial compact density and grain size, (2) chemical composition of the source, and (3) the temperature and pressure of the process. The application of the technique to the synthesis of SiC and diamond with Si, Ge, and different metals. Results of the in-situ investigation of the synthesis process by synchrotron X-ray diffraction technique will be presented.

Gierlotka, S.↗

DOE OSTI2025

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↗

DOE OSTI2026

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 ↗

DOE OSTI2026

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↗

DOE OSTI2026

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,↗

DOE OSTI2025

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↗

NASA NTRS1999

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.↗

DOE OSTI2024

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↗

DOE OSTI2025

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↗

DOE OSTI2025

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↗

DOE OSTI2025

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↗

DOE OSTI2025

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↗

NASA NTRS1987

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↗