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At least 1,459 records · Page 81
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Kinetic analyses for solid-state phase transition of metastable amorphous-AlO x (2.5 < x ≤ 3.0) nanostructures into crystalline alumina polymorphs

Solid-solid phase change materials (SS-PCMs) hold promise for energy storage/dissipation in batteries and energetic materials. Yet, phase change kinetics for SS-PCMs undergoing metastable to semi-stable/stable phase transformations remain relatively ill-studied because trapping metastable phases remain challenging. Recently, we demonstrated the kinetic entrapment and stabilization of a highly disordered and amorphous Al-oxide phase m-AlO x @C (x~2.5-3.0) via laser ablation synthesis in solution (LASiS). We report here, to our knowledge, the first chemical kinetics analysis for S-S phase transition of the m-AlO 3 @C nanocomposites (< 5–8 nm sizes) into semi-stable equilibrium alumina phases (θ/γ-Al 2 O 3 ) via disproportionation reaction, while releasing excess trapped gases. Our results indicate the atomic density of the AlO 3 structures to be ~5–10 times less than that of the final Al 2 O 3 phases, which led to the hypothesis of a volume shrinkage process during their phase transition. Temperature-dependent X-ray diffraction studies reveal the high-temperature phase transition for m-AlO 3 → θ/γ-Al 2 O 3 to follow contracting volume kinetics model, thereby validating our earlier hypothesis. Using the geometric volume contraction model, reaction kinetics analyses from Arrhenius plots reveal the activation energy barrier for the phase transition to be ~270±11 kJ/mol. This makes the activation energy barrier nearly identical to the oxidation of micron-sized Al particles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Highly Al-doped TiO{sub 2} nanoparticles produced by Ball Mill Method: structural and electronic characterization

Highlights: • Highly Al-doped TiO{sub 2} nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO{sub 2} nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy. The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti{sup 4+} ions by Al{sup 3+} in the TiO{sub 2} lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

9 T high magnetic field annealing effects on FeN bulk sample

α″-Fe{sub 16}N{sub 2} has been suggested as a promising candidate for future rare-earth-free magnets. In this paper, we report to use high magnetic field (9 T) assisted post-annealing process to enhance the Fe{sub 16}N{sub 2} phase formation in FeN bulk rod samples during the α′ → α″ phase transformation and thus improve its magnetic properties. It was found by X-ray Diffraction measurement that the volume ratio of Fe{sub 16}N{sub 2} phase was increased up to 22%, which corresponds to an increase in the amount of transformation from α′ → α″ up to 78%. Also, the saturation magnetization (M{sub s}) of the prepared FeN rod sample was increased to 227 emu/g with its coercivity up to 376 Oe at room temperature. A working mechanism for the high field assisted post-annealing process was presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

ζ-Glycine: insight into the mechanism of a polymorphic phase transition

Glycine is the simplest and most polymorphic amino acid, with five phases having been structurally characterized at atmospheric or high pressure. A sixth form, the elusive ζ phase, was discovered over a decade ago as a short-lived intermediate which formed as the high-pressure ϵ phase transformed to the γ form on decompression. However, its structure has remained unsolved. We now report the structure of the ζ phase, which was trapped at 100 K enabling neutron powder diffraction data to be obtained. The structure was solved using the results of a crystal structure prediction procedure based on fully ab initio energy calculations combined with a genetic algorithm for searching phase space. We show that the fate of ζ-glycine depends on its thermal history: although at room temperature it transforms back to the γ phase, warming the sample from 100 K to room temperature yielded β-glycine, the least stable of the known ambient-pressure polymorphs.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Deformation behavior of additively manufactured GP1 stainless steel

In-situ neutron diffraction measurements were performed in this paper during heat-treating and uniaxial loading of additively manufactured (AM) GP1 material. Although the measured chemical composition of the GP1 powder falls within the composition specifications of 17-4 PH steel, a fully martensitic alloy in the wrought condition, the crystal structure of the as-built GP1 material is fully austenitic. Chemical analysis of the as-built material shows high oxygen and nitrogen content, which then significantly decreased after heat-treating in a vacuum furnace at 650 °C for one hour. Significant austenite-to-martensite phase transformation is observed during compressive and tensile loading of the as-built and heat-treated material with accompanied strengthening as martensite volume fraction increases. During loading, the initial average phase stress state in the martensite is hydrostatic compression independent of the loading direction. Finally, preferred orientation transformation in austenite and applied load accommodation by variant selection in martensite are observed via measurements of the texture development.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Phase transitions of α-quartz at elevated temperatures under dynamic compression using a membrane-driven diamond anvil cell: Clues to impact cratering?

Coesite and stishovite are high-pressure silica polymorphs known to have been formed at several terrestrial impact structures. They have been used to assess pressure and temperature conditions that deviate from equilibrium formation conditions. Here in this paper, we investigate the effects of nonhydrostatic, dynamic stresses on the formation of high-pressure polymorphs and the amorphization of α-quartz at elevated temperatures. The obtained disequilibrium states are compared with those predicted by phase diagrams derived from static experiments under equilibrium conditions. We analyzed phase transformations starting with α-quartz in situ under dynamic loading utilizing a membrane-driven diamond anvil cell. Using synchrotron powder X-ray diffraction, the phase transitions of SiO 2 are identified up to 77.2 GPa and temperatures of 1160 K at compression rates ranging between 0.10 and 0.37 GPa s -1 . Coesite starts forming above 760 K in the pressure range between 2 and 11 GPa. At 1000 K, coesite starts to transform to stishovite. This phase transition is not completed at 1160 K in the same pressure range. Therefore, the temperature initiates the phase transition from α-quartz to coesite, and the transition from coesite to stishovite. Below 1000 K and during compression, α-quartz becomes amorphous and partially converts to stishovite. This phase transition occurs between 25 and 35 GPa. Above 1000 K, no amorphization of α-quartz is observed. High temperature experiments reveal the strong thermal dependence of the formation of coesite and stishovite under nonhydrostatic and disequilibrium conditions.

58 GEOSCIENCES↗
DOE OSTI2021

Electronic Structure, Chemical Bonding and Electrocatalytic Activity of Novel Ba(Fe0.7Ta0.3)O3-d Compounds

Ba(Fe0.7Ta0.3)O3-d (BFTO) compounds were synthesized using conventional, high-temperature solid-state ceramic reaction method by varying the sintering temperature (Ts=1200-1350 °C). The crystal structure, electronic structure and electrocatalytic activity of BFTO compounds were evaluated. Processing temperature induced phase transformations and structural quality influences the electronic structure and electrocatalytic activity of BFTO compounds. At Ts=1200 oC, Ba(Fe0.7Ta0.3)O3-d stabilizes in mixed phase of orthorhombic + rhombohedral phase (Amm2 + R3m). With increasing Ts (=1250 oC), Ba(Fe0.7Ta0.3)O3-d ceramics stabilize in tetragonal + rhombohedral [P4mm + R3m] mixed phase with a variation in the quantity of respective phases. High-resolution X-ray photoelectron spectroscopy of constituent elements, namely, Ba 3d, Fe2p, Ta 4f and O 1s reveal the electronic structure changes due to changes in chemical environment resulted from structural transformation. The electrocatalytic activity of BFTO was evaluated towards hydrogen evolution reaction (HER) and oxygen reduction reaction (ORR). Though all the samples demonstrated appreciable electrocatalytic properties, the best electrochemical catalytic activity was shown by BFTO samples sintered at 1350 °C. BFTO-1350 oC showed an onset potential of -0.690 V vs. RHE for HER and an onset potential of 0.73 V vs. RHE for ORR indicating its significant electrocatalytic performance. A general increase in activity with sintering temperature is potentially due to the improved structural quality of the BFTO ceramics. In addition to offering the fundamental insights into solid state materials based on doped BaTiO3 for electrocatalysis, the present work may contribute to the design and development of materials for high-temperature electrocatalytic converters.

Ba(Fe0.7Ta0.3)O3-d, Phase Transformation↗
DOE OSTI2022

Thermal conversion in air of rare-earth fluorides to rare-earth oxyfluorides and rare-earth oxides

Phase transformations of seven different rare-earth fluorides (i.e., REF3) where RE = La, Ce, Pr, Nd, Tm, Yb, Lu at temperatures ranging from 400–1400°C in air were investigated with X-ray diffraction. All of the REF3 compounds first transformed to oxyfluorides and then to oxides, with the exception of CeF3, which transformed directly to an oxide. This study focuses on the phase transitions of REF3 to REOx by simple heat-treatment processes in air and shows plausibility to remove RE elements from fluoride salt streams from molten salt reactors through fluoride-to-oxyfluoride or fluoride-to-oxide conversion mechanisms, which will result in precipitation. This could be used to remove fission product poisons from molten salt reactor waste streams. A waste form option for the resulting REOx products is lanthanide aluminoborosilicate (LABS) glass. To demonstrate this NdF3 was converted to Nd2O3 and immobilized in a LABS glass.

oxyfluoride, molten salt reactors, fluoride salt w↗
DOE OSTI2013

High-temperature X-ray analysis of phase evolution in lithium ion conductor Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3}

Series of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass ceramic samples were prepared in this work through the change of heat treatment temperature from 650 to 1050 °C. The structures of glass ceramic samples were characterized by means of high temperature X-ray diffraction and Field Emission Scanning Electron Microscope. And the lithium ionic conductivity was analyzed through AC impedance spectroscopy. Through heat treatment at 850 °C for 4 h for the base glass sample, we obtained a maximum conductivity of 5.8 × 10{sup −4} S/cm at room temperature. - Graphical Abstract: High temperature X-ray diffraction (HT-XRD) and Rietveld refinement of Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} (LAGP) glass-ceramics were recorded to investigate the phase transformation, cell parameters and the mass fraction of each crystal phase, which occur in the glass to glass-ceramics process during different crystallization temperatures. The relationship between the average grain size and conductivity that originate from and relate to the crystallization temperature was analyzed by SEM micrograph and AC impedance spectroscopy. - Highlights: • Li{sub 1.5}Al{sub 0.5}Ge{sub 1.5}(PO{sub 4}){sub 3} glass-ceramics were prepared from as-prepared glass. • The phases decomposition and mass fraction of each phase were analyzed by HT-XRD. • Conductivity is relate to grain size that influenced by crystallization temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Crystal Chemistry and Electrochemistry of Li x Mn 1.5 Ni 0.5 O 4 Solid Solution Cathode Materials

For ordered high-voltage spinel LiMn 1.5 Ni 0.5 O 4 (LMNO) with the P4 3 2 1 symmetry, the two consecutive two-phase transformations at ~4.7 V (vs Li + /Li), involving three cubic phases of LMNO, Li 0.5 Mn 1.5 Ni 0.5 O 4 (L 0.5 MNO), and Mn 1.5 Ni 0.5 O 4 (MNO), have been well-established. Such a mechanism is traditionally associated with poor kinetics due to the slow movement of the phase boundaries and the large mechanical strain resulting from the volume changes among the phases, yet ordered LMNO has been shown to have excellent rate capability. In this paper, we show the ability of the phases to dissolve into each other and determine their solubility limit. We characterized the properties of the formed solid solutions and investigated the role of non-equilibrium single-phase redox processes during the charge and discharge of LMNO. Finally, by using an array of advanced analytical techniques, such as soft and hard X-ray spectroscopy, transmission X-ray microscopy, and neutron/X-ray diffraction, as well as bond valence sum analysis, the present study examines the metastable nature of solid-solution phases and provides new insights in enabling cathode materials that are thermodynamically unstable.

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

Direct extraction of lithium from ores by electrochemical leaching

With the rapid increase in lithium consumption for electric vehicle applications, its price soared during the past decade. To secure a reliable and cost-effective supply chain, it is critical to unlock alternative lithium extraction resources beyond conventional brine. In this study, we develop an electrochemical method to directly leach lithium from α-phase spodumene. We find the H 2 O 2 promoter can significantly reduce the leaching potential by facilitating the electron transfer and changing the reaction path. Upon leaching, β-phase spodumene shows a typical phase transformation to HAlSi 2 O 6 , while leached α-phase remains its original crystal phase with a lattice shrinkage. To demonstrate the scale-up potential of electrochemical leaching, we design a catalyst-modified high-throughput current collector for high loading of suspended spodumene, achieving a leaching current of 18 mA and a leaching efficiency of 92.2%. Electrochemical leaching will revolutionize traditional leaching and recycling processes by minimizing the environmental footprint and energy consumption.

25 ENERGY STORAGE↗
DOE OSTI2024

Cubic and hexagonal boron nitride phases and phase boundaries

We used temperature-dependent spark plasma sintering to induce phase transformations of metastable 3D c-BN to mixed-phase 3D/2D c-BN/h-BN and ultimately to the stable 2D h-BN phase at high temperature, useful for extreme-temperature technology.

Materials Science↗
NASA NTRS1972

Elasticity of some mantle crystal structures. I - Pleonaste and hercynite spinel.

The elasticity of high-pressure mantle phases can be characterized by using data for chemically similar crystal compounds. The single-crystal elastic constants are determined as a function of pressure and temperature for pleonaste spinel and at room conditions for hercynite spinel. The bulk modulus increases from 1.95 Mb for pleonaste spinel to 2.10 Mb for hercynite spinel. Low or negative values of the pressure derivatives of shear constants are characteristic of the spinel structure and imply a low kinetic barrier to phase transformations and diffusion. Compressional and shear velocities of the spinel phase of olivine are estimated as a function of mean atomic weight by using the pleonaste and hercynite data.

Wang, H.↗
NASA NTRS1983

Temperatures of shock-induced shear instabilities and their relationship to fusion curves

New emission spectra for MgO and CaAl2Si2O8 (glass) are observed from 430 to 820 nm. Taken with previous data, it is suggested that transparent solids display three regimes of light emission upon shock compression to successively higher pressures: (1) characteristic radiation such as observed in MgO and previously in other minerals, (2) heterogeneous hot spot (greybody) radiation observed in CaAl2Si2O8 and previously in all transparent solids undergoing shock-induced phase transformations, and (3) blackbody emission observed in the high pressure phase regime in NaCl, SiO2, CaO, CaAl2Si2O8, and Mg2SiO4. The onset of the second regime may delineate the onset of shock-induced polymorphism whereas the onset of the third regime delineates the Hugoniot pressure required to achieve local thermal equilibrium in the shocked solid. It is also proposed that the hot spot temperatures and corresponding shock pressures determined in the second regime delineate points on the fusion curves of the high pressure phase.

Schmitt, D. R.↗
NASA NTRS1987

Phase closure with a rotational shear interferometer

A simple and efficient way is proposed for achieving phase closure in an optical telescope (to enable recovering Fourier transform phases that would otherwise be corrupted by atmospheric and instrumental errors), by means of rotational shear interferometry. In a rotational shear interferometer, one images the telescope aperture onto the interferometer and then interferes the aperture with itself in a rotated orientation. To achieve the maximum frequency content permitted by the telescope, the shear has to be 180 deg, but better dynamic range and SNR are possible for lower frequencies. Drawbacks of the proposed method compared to radio astronomy are noted, and different approaches are indicated as to how to collect and use the phase closure data. Phase closure can be realized on existing telescopes and existing interferometers with special modifications. Although not all base lines are possible, the extra constraints provided by the closure phases greatly reduce the ambiguity now existing in phaseless image reconstruction.

Ribak, Erez↗
NASA NTRS1990

Shock induced polymorphic transition in quartz, carbon, and boron nitride

The model proposed by Ahrens (1988) to explain the mechanism of the polymorphism in silicates is revised, and the revised model is applied to the quartz/stishovite, graphite/diamond, and graphite-boron nitride (g-BN) phase transformations. In this model, a key assumption is that transformation to a high-density amorphous or possibly liquid phase which rapidly crystallized to the high-pressure phase is triggered by the high temperatures in the shear band and upon crossing the metastable extension of a melting curve. Good agreement between the calcualted results and published data is obtained. The present theory predicts the standard entropy for cubic BN to be 0.4-0.5 J/g K.

Tan, Hua↗
DOE OSTI2021

Martensitic transformation in superlattices of two non-transforming metals

A number of studies have shown that the coherent integration of a second non-transforming phase in martensitic materials results in unprecedented thermo-mechanical properties. We demonstrate the possibility of martensitic transformation by epitaxially combining two non-transforming materials, Mg (hexagonal closed packed) and MgLi (body centered cubic). Density functional theory calculations predict that MgLi/Mg superlattices undergo a transformation crystallographically equivalent to MgSc alloys and can be expected to result in finite temperature shape memory behavior. We predict the zero-temperature energy of the martensite phase to be 9.3 meV/atom lower than austenite for a 50–50 at. % MgLi/Mg nanolaminate, which is expected to result in a martensitic transformation temperature of approximately 150 K. This energy difference can be tuned between 4.9 and 18.1 meV/atom by varying the fraction of the pure Mg phase in the superlattice, potentially enabling the transformation from cryogenic to room and higher temperatures. While Li diffusion might limit the applications of the systems proposed, this work opens the door to a new approach to create martensitic materials.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗