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At least 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Nanotwinned alloys under high pressure

Nanotwinned alloys are of interest due to their high strength and ductility, but twin boundaries may not be stable under shear. Computational studies indicate that high hydrostatic pressure may suppress detwinning mechanisms. Here, in this study, we investigate the microstructural changes of nanotwinned-nanocrystalline copper-nickel and Inconel 725 alloys under quasi-hydrostatic pressures up to 50 gigapascals (GPa). The alloys are compressed in a diamond anvil cell. In-situ x-ray diffraction (XRD) and ex-situ transmission electron microscopy (TEM) were employed to monitor microstructural changes. Twin boundary deformation and grain growth occur at 11.4 GPa quasi-hydrostatic pressure in the copper-nickel alloy. Molecular dynamics (MD) simulations reveal that hydrostatic pressure causes elevated local shear stress at grain boundaries, which leads to atomic rearrangements. A superposition of hydrostatic and deviatoric pressures lead to partial dislocation mediated twin boundary migration. In contrast, the Inconel 725 alloy showed stable twin and grain boundaries up to a quasi-hydrostatic pressure of 12.7 GPa. Texture, high solid solution strengthening, and low stacking fault energy are hypothesized to the enhanced microstructural stability in Inconel 725.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Formation of hydrocarbons favored by high pressure at subduction zone conditions

Subduction zones enable carbon transport to the deep Earth. Inorganic and organic carbon in fluids released from the subducted slab are important in water-rock interactions. However, the potential role of reduced carbon species in fluids during subduction is still unclear. In particular, the pressure, temperature, and oxidation state conducive to the formation of fluid hydrocarbons are poorly understood. Here we focused on the role of pressure influencing the formation of hydrocarbons using diamond anvil cell experiments starting with 0.5 M Ca-acetate solutions over a broad range of pressures, from 1.6 to 4.6 GPa at temperatures of 300 and 350°C. Droplets of immiscible hydrocarbon fluid coexisting with aqueous carbonate or bicarbonate and crystals of calcite or aragonite were formed at peak pressure and temperature conditions in the experiments. Furthermore, greater quantities of hydrocarbons formed at higher pressure as revealed by measuring the in situ volume percent of the droplets. Measurement of the in situ Raman spectra of the co-existing aqueous solutions and analysis of the peak area ratios of acetate to HCO 3 – showed faster decrease at higher pressure, which indicated that the reactions forming hydrocarbons were accelerated by pressure. Compared to previous Na-acetate experiments at 300°C and 3.0 GPa, this study found hydrocarbons that were more methane-rich and had more propane and less isobutane. In experiments at 350°C, isobutane transformed to one or more aromatic hydrocarbons in an immiscible fluid. The air-dried aromatic hydrocarbons were measured using a UV laser, and show peaks of bitumen. Overall, our study supports the hypothesis that high pressures and high temperatures facilitate the possible occurrence of immiscible hydrocarbon fluids in the deep carbon cycle.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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 OSTI2024

A novel means to generate high pressure

Diamond anvil cells are the most popular means of generating pressures above 2 GPa. However, in many experiments, such as nuclear magnetic resonance and x-ray absorption, the metallic pressurizing gasket (which confines much of the sample) represents an occluding barrier that requires a low Z gasket material (e.g., Be), a split gasket, or other means to enable better coupling of the sample to electromagnetic radiation. In this paper, we demonstrate a novel method for generating high pressures that confines the sample just above the plane of the gasket by using a diamond with a laser hole drilled into the center of the tip. The sample is then confined by the hole, which is sealed by a flat gasket that fits over the hole. When load is applied to the diamonds, metal flows from the deformed gasket into the hole thereby pressurizing the sample similarly to how a piston pressurizes gas inside a cylinder. The pressurized sample is above the metallic gasket plane just inside the tip of the diamond, and thus easily accessible via x rays or visible light that skims just above the plane of the gasket providing an enhanced aperture of radiation collection. Furthermore, we have demonstrated the utility of this method by obtaining Raman spectra of SnC 2 O 4 and x-ray diffraction spectra of seleno-DL-cystine, all at high pressures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2024

Extending carbon chemistry at high-pressure by synthesis of CaC 2 and Ca 3 C 7 with deprotonated polyacene- and para-poly(indenoindene)-like nanoribbons

Metal carbides are known to contain small carbon units similar to those found in the molecules of methane, acetylene, and allene. However, for numerous binary systems ab initio calculations predict the formation of unusual metal carbides with exotic polycarbon units, [C 6 ] rings, and graphitic carbon sheets at high pressure (HP). Here we report the synthesis and structural characterization of a HP-CaC 2 polymorph and a Ca 3 C7 compound featuring deprotonated polyacene-like and para-poly(indenoindene)-like nanoribbons, respectively. We also demonstrate that carbides with infinite chains of fused [C6] rings can exist even at conditions of deep planetary interiors (~140 GPa and ~3300 K). Hydrolysis of high-pressure carbides may provide a possible abiotic route to polycyclic aromatic hydrocarbons in Universe.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Accelerating the Scalability of PrintCast structures using High Pressure Die Casting

PrintCast composites are fabricated by infiltrating a metal mesh or preform (e.g., an additively-manufactured 316L lattices) with molten metal of a lower melting temperature (e.g., A380 aluminum). The resulting PrintCast composite has been shown in the literature to produce diverse and unique mechanical properties that are controllable at the local or global level by adjusting volume-fraction and/or topology of the preforms geometry and overall volume fraction. Although promising mechanical and thermal properties have been achieved at the laboratory scale level, the scalability from laboratory to full scale components has been limited using conventional casting infiltration. This work highlights how using high pressure die casting can significantly advance the development and eventual deployment of PrintCast approaches at large scales. We have successfully produced 9-inch by 6-inch by 1-inch thick PrintCast 316L stainless steel/A380 aluminum “bricks” via high pressure die casting. Initial findings show excellent infiltration and production capability. The resulting approach demonstrates the scalability and manufacturability of hybrid cost effective metal-metal matrix composites at larger length scales with high quality infiltration results.

Splitter, Derek↗
DOE OSTI2022

Charge Reservoirs in an Expanded Halide Perovskite Analog: Enhancing High–Pressure Conductivity through Redox–Active Molecules

As halide perovskites and their derivatives are being developed for numerous optoelectronic applications, controlling their electronic doping remains a fundamental challenge. Herein, we describe a novel strategy of using redox-active organic molecules as stoichiometric electron acceptors. The cavities in the new expanded perovskite analogs (dmpz)[Sn 2 X 6 ], (X=Br – (1Br) and I – (1I)) are occupied by dmpz 2+ (N,N'-dimethylpyrazinium), with the LUMOs lying ca. 1 eV above the valence band maximum (VBM). Compressing the metal-halide framework drives up the VBM in 1I relative to the dmpz LUMO. The electronic conductivity increases by a factor of 105 with pressure, reaching 50(17) S cm –1 at 60 GPa, exceeding the high-pressure conductivities of most halide perovskites. This conductivity enhancement is attributed to an increased hole density created by dmpz 2+ reduction. Lastly, this work elevates the role of organic cations in 3D metal-halides, from templating the structure to serving as charge reservoirs for tuning the carrier concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Computational flow modeling of triply periodic minimal surfaces as feed channel spacers in ultra-high pressure reverse osmosis applications

Triply periodic minimal surfaces (TPMS) are a special class of mathematical surfaces characterized by a high surface area-to-volume ratio. They have generated considerable interest in fields such as acoustics, heat transfer, and membrane-based filtration processes. This study evaluates the performance of four different TPMS designs—Schoen Gyroid, Schoen Crossed Layers of Parallels (CLP), Schoen Transverse Crossed Layers of Parallels (tCLP), and Schwarz-Primitive—when used as feed channel spacers under ultra-high pressure reverse osmosis (UHPRO) conditions, at approximately 200 bar. Our experimentally validated computational fluid dynamics model reveal different flow patterns within the feed channels for each of the four TPMS designs, leading to varying hydrodynamic and permeation properties. Under the simulated UHPRO conditions, the Gyroid and tCLP designs yield up to a 23% increase in average permeate velocity and a 14% reduction in average membrane-surface concentration relative to a non-woven spacer of the same porosity. Furthermore, the enhanced performance comes with an increased feed channel pressure drop, although it only constitutes less than 4% of the operating pressure when extrapolated for a meter-long membrane module. Additionally, the study analyzes the effects of varying inlet velocity and spacer porosity on membrane performance. Overall, this research provides valuable insights into the potential use of TPMS spacers in UHPRO applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

A new capability for investigating the structure and dynamics of liquids at high pressures

Water and aqueous solutions are critical to many areas of science and technology. As a result, tremendous effort has been devoted to understanding them in detail. Despite over a century of research, fundamental questions about water and aqueous solutions remain unanswered. However, an intriguing possibility – that liquid water can exist in two thermodynamically distinct states – has emerged as the most likely explanation. The problem is that experimental confirmation of this hypothesis requires experiments on water at high pressures and low temperatures, conditions in which liquid water only exists briefly before turning into crystalline ice. This project investigated the feasibility of developing a new capability for study water and aqueous solutions under these challenging conditions. The physical constraints, such as the timescales for crystallization and thermal diffusion in supercooled water, were evaluated along with their impact on the design criteria for the instrument. Several basic design options were considered that could meet the technical requirements. The options were also evaluated with respect to their use of commercially available equipment versus the need for custom designs or in-house development. The project identified two viable options to pursue. The first option would use a high-pressure syringe pump in conjunction with fused silica (or sapphire) capillaries. The second option would use a diamond anvil cell. These options can both be used with optical spectroscopies, such as Raman or Infrared.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2024

Direct numerical simulation of a high-pressure hydrogen micromix combustor: Flame structure and stabilisation mechanism

A high-pressure hydrogen micromix combustor has been investigated using direct numerical simulation with detailed chemistry to examine the flame structure and stabilisation mechanism. The configuration of the combustor was based on the design by Schefer et al., using numerical periodicity to mimic a large square array. A precursor simulation of an opposed jet-in-crossflow was first conducted to generate appropriate partially-premixed inflow boundary conditions for the subsequent reacting simulation. The resulting flame can be described as an predominantly-lean inhomogeneously-premixed lifted jet flame. Five main zones were identified: a jet mixing region, a core flame, a peripheral flame, a recirculation zone, and combustion products. The core flame, situated over the jet mixing region, was found to burn as a thin reaction front, responsible for over 85% of the total fuel consumption. The peripheral flame shrouded the core flame, had low mean flow with high turbulence, and burned at very lean conditions (in the distributed burning regime). It was shown that turbulent premixed flame propagation was an order-of-magnitude too slow to stabilise the flame at these conditions. Stabilisation was identified to be due to ignition events resulting from turbulent mixing of fuel from the jet into mean recirculation of very lean hot products. Ignition events were found to correlate with shear-driven Kelvin-Helmholtz vortices, and increased in likelihood with streamwise distance. At the flame base, isolated events were observed, which developed into rapidly burning flame kernels that were blown downstream. Further downstream, near-simultaneous spatially-distributed ignition events were observed, which appeared more like ignition sheets. The paper concludes with a broader discussion that considers generalising from the conditions considered here.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Observation of Thermally Induced Piezomagnetic Switching in Cu 2 OSeO 3 Polymorph Synthesized under High-Pressure

A polymorph of Cu 2 OSeO 3 with the distorted kagome lattice is successfully obtained using the high-pressure synthesis technique (Cu 2 OSeO 3 -HP). The structural analysis using X-ray and neutron powder diffraction suggests that the tetrahedral Cu 2+ clusters [similar to those in Cu 2 OSeO 3 ambient-pressure phase (Cu 2 OSeO 3 -AP)] exist in Cu 2 OSeO 3 -HP but with three symmetry inequivalent sites. No structural change is observed between 1.5 K and the room temperature. The complex magnetic H-T phase diagram is established based on the temperature- and field-dependent magnetization data, indicating two distinct antiferromagnetic phases at low and intermediate temperatures, in addition to the higher-temperature spin-glass-like phase. The low temperature phase is identified by neutron powder diffraction refinements as a canted noncollinear antiferromagnetic order with a weak ferromagnetic component along the b-axis. Size of the refined ordered moment is ≈1.00(4) µ B in Cu 2 OSeO 3 -HP, indicating a large enhancement compared to that of Cu 2 OSeO 3 -AP (≈0.61 µ B ). By applying a uniaxial stress, finite enhancement of weak ferromagnetic component in the noncollinear antiferromagnetic phase in Cu 2 OSeO 3 -HP is observed, which is the clear evidence of the piezomagnetic effect. Interestingly, the sign of the induced magnetization changes on heating from the low-temperature to the intermediate-temperature phases, indicating a novel piezomagnetic switching effect in this compound.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Zeolitic-Imidazolate Framework Derived Intermetallic Nickel Zinc Carbide Material as a Selective Catalyst for CO 2 to CO Reduction at High Pressure

The conversion of CO 2 into CO is an important step in CO 2 utilization to achieve clean fuels and value-added chemicals. Herein, we explored the pyrolysis of zeolitic imidazolate framework-8 (ZIF-8) loaded with different amounts of Ni 2+ to obtain Ni-Zn carbide (Ni 3 ZnC) embedded in N-doped carbon. Ni is present in the intermetallic compound, while Zn excess remains on the N-doped carbon. The Ni 3 ZnC phase catalyzes the selective hydrogenation of CO 2 into CO via the reverse water gas shift reaction, reaching 100 % CO selectivity at ~30 % CO 2 conversion at 450 °C and atmosphere pressure (CO 2 :H 2 =1:4, GHSV=30000 mL g cat -1 h -1 ). The methanation reaction of CO 2 /CO, which is usually favored over Ni catalysts, is suppressed. The selectivity to CO at the expense of CH 4 is related to the stability of chemisorbed CO in the Ni 3 ZnC surface, which is lower compared to Ni surfaces. The Ni 3 ZnC@NC catalyst is selective towards CO over a wide range of conditions, including high pressure, that is usually required for the conversion of CO to hydrocarbons and alcohols via the Fisher-Tropsch synthesis (FTS) process. Contrarily, a classical Ni/SiO 2 catalyst prepared by impregnation produces CH 4 under high pressure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Ignition delay time and speciation of dibutyl ether at high pressures

Dibutyl ether (DBE) is a promising biofuel due to its high cetane number (~ 100) and high volumetric energy density (31.6 MJ/L). It could either be used directly in compression ignition engines or blended with other conventional or renewable fuels. Oxidation and pyrolysis kinetics of DBE are not well known, particularly at high pressures. In this work, we have experimentally investigated the chemical kinetics of DBE in three domains: (a) ignition delay time measurements in a rapid compression machine over T = 550–650 K, P = 10, 20, 40 bar, φ = 0.5, 1; (b) ignition delay time measurements in a shock tube over T = 900–1300 K, P = 20, 40 bar, φ = 0.5, 1; (c) laser-based carbon monoxide speciation measurements in a shock tube during DBE pyrolysis and oxidation over T = 1100–1400 K, P = 20 bar. Pressure time-histories measured in RCM experiments exhibited unique 3-stage and 4-stage ignition behavior predominantly at fuel-lean conditions. Experimental data were compared with the predictions of two recent chemical kinetic models of DBE. Sensitivity analyses were carried out to identify key reactions which may have caused the discrepancy between experiments and simulations. We found that the rate of decomposition of DBE may need to be revisited to improve the oxidative and pyrolytic predictions of DBE kinetic model.

09 BIOMASS FUELS↗
DOE OSTI2021

Nanocolumnar Pt:Ni Alloy Thin Films by High Pressure Sputtering for Oxygen Reduction Reaction

Self-supported nanocolumnar Pt:Ni thin films (TFs) with varying Pt:Ni atomic ratios and Pt mass loadings were produced on a microporous layer (MPL)-like surface composed of carbon particles by high pressure sputtering and examined as oxygen reduction reaction (ORR) electrocatalysts for polymer electrolyte membrane fuel cells. Cauliflower-like microstructures were observed from scanning electron microscopy imaging. Various Pt:Ni atomic ratios were obtained by simply changing the relative deposition power between Pt and Ni source and investigated by X-ray diffraction and quartz crystal microbalance analysis. Additionally, electrochemical characterization of the Pt:Ni-TF/MPL-like-layer/glassy-carbon samples was conducted through benchtop cyclic voltammetry and rotating disk electrode measurements. The electrochemically active surface area (ECSA) was found to be between 22–42 m 2 g -1 for different Pt:Ni atomic ratios. Lower Pt mass loadings exhibited a higher ECSA and the catalytic activity of all Pt:Ni ratios increased with the increase in Pt mass loading. The ORR activity of the Pt:Ni-TFs increased in the order of 3:1 < 1:1 < 1:3 with exhibiting a specific activity of 1781 μA cm -2 and mass activity of 0.66 A mg -1 for the Ni-rich film with 1:3 ratio. The catalytic performance of Pt:Ni-TFs were higher than traditional high surface area carbon supported Pt nanoparticles, elemental Pt nanorods, and Pt-Ni nanorods.

08 HYDROGEN↗
DOE OSTI2024

Friction stir processing: A thermomechanical processing tool for high pressure die cast Al-alloys for vehicle light-weighting

This study uses friction stir processing (FSP) for thermomechanical processing of high-pressure die-casting (HPDC) to modify microstructure and improve mechanical properties. FSP is carried out on two different HPDC aluminum alloys: (a) general-purpose, high-iron, HPDC A380 alloy and (b) premium quality, low-iron HPDC Aural-5 alloy in thin wall, flat plate geometry. Subsequent mechanical testing shows ~30 % and ~65 % enhancement in yield strength and tensile ductility. In addition, FSP leads to ~10 times improvement in fatigue life for A380 alloy and ~70 % improvement in fracture toughness for Aural-5 alloy. These findings emphasize the capability of FSP to modify the microstructure of HPDC Al-alloys-based structural components so that they can demonstrate a good combination of strength, ductility, fracture toughness, and high fatigue properties for long-term durability and reliability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Investigation of species-mass diffusion in binary-species boundary layers at high pressure using direct numerical simulations

Here, direct numerical simulations of single-species and binary-species temporal boundary layers at high pressure are performed with special attention to species-mass diffusion. The working fluids are nitrogen or a mixture of nitrogen and methane. Mean profiles and turbulent fluctuations of mass fraction show that their qualitative characteristics are different from those of streamwise velocity and temperature, due to the different boundary conditions. In a wall-parallel plane near the wall, the streamwise velocity and temperature have streaky patterns and the fields are similar. However, the mass fraction field at the same location is different from the streamwise velocity and temperature fields indicating that species-mass diffusion is not similar to the momentum and thermal diffusion. In contrast, at the centre and near the edge of the boundary layer, the mass fraction and temperature fields have almost the same pattern, indicating that the similarity between thermal and species-mass diffusion holds away from the wall. The lack of similarity near the wall is traced to the Soret effect that induces a temperature-gradient-dependent species-mass flux. As a result, a new phenomenon has been identified for a non-isothermal binary-species system – uphill diffusion, which in its classical isothermal definition can only occur for three or more species. A quadrant analysis for the turbulent mass flux reveals that near the wall the Soret effect enhances the negative contributions of the quadrants. Due to the enhancement of the negative contributions, small species-concentration fluid tends to be trapped near the wall.

42 ENGINEERING↗
DOE OSTI2021

Spectroscopic Investigation of the High-Pressure Behavior of Aliphatic Hydrocarbon: Implications for Planetary Processes

Octadecane (C 18 H 38 ) is an aliphatic hydrocarbon that is abundant in carbonaceous chondritic meteorites. It is debated whether these hydrocarbons found in the meteorite are pristine or are a result of subsequent modifications as these meteorites are delivered to the Earth. It is well-known that meteorites are often subjected to extreme pressures and temperatures upon entering the Earth’s atmosphere. To explore the behavior of octadecane at high pressures, that is, how its molecular structure responds to compression, we use a diamond anvil cell in conjunction with Raman spectroscopy. Here, we find that at room temperatures, upon compression to ~5 GPa, a linear-chain octadecane molecule transforms into a bent-chain configuration. Similar transitions from linear to a bent configuration in other hydrocarbons have been documented. We find a linear correlation between the transition pressure from linear to bent configuration, and the chain length of the alkane, that is, longer chain lengths, is likely to be less stable in the linear configuration under compression. These kinks in the bent-chain configuration are likely sites for the dissociation of the longer chain hydrocarbons to smaller hydrocarbons. The octadecane sample examined in this study did not undergo any additional transition to the highest pressure (~18 GPa) explored in this study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Microstructural evolution and intermetallic formation in Zn-3Mg (wt%) powder mixture processed by high-pressure torsion

Severe plastic deformation (SPD) techniques have been used extensively over the past 40 years for producing strong metals and alloys. High-pressure torsion (HPT) is one of the most promising SPD techniques for achieving high strength through nanoscale grain refinement and phase transformation. In this research, a mixture of pure zinc (Zn) and magnesium (Mg) powders, Zn-3Mg (wt%), was HPT-processed under a pressure of 6 GPa for 1, 5, 10, 20, and 30 turns at room temperature to achieve a high strength biodegradable material. In order to understand the effects of pre-consolidation on the resulting microstructure and hardness, HPT processing was performed on loose powders placed in the die and also on a pre-compacted powder mixture and the resulting HPT disks were characterized by X-ray diffraction, scanning electron microscopy, atom probe tomography, and Vickers microhardness. In both cases, the HPT disk microstructures contained nanoscale grains, and stable and metastable strain-induced intermetallics, but an unusual softening appeared at large shear strains. Grain size, grain morphology, and the formation of different intermetallics were analyzed to explain the unusual hardness distribution, and it was found that an inverse Hall-Petch relationship between hardness and grain size exists. It is suggested that thermally-activated phenomena such as grain boundary sliding contributed to the strain-induced softening of this nano-structured biomaterial due to its low melting point. Finally, the current results are compared with those for HPT-processed cast alloys and hybrids of the same composition.

36 MATERIALS SCIENCE↗