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Results for “High pressure X-ray diffraction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1982

X-ray diffraction from high pressure Ge using synchrotron radiation

The high pressure structural phase transition in Ge has been studied using the energy dispersive X-ray diffraction technique and a synchrotron radiation source. Ge was observed to transform to the beta-Sn tetragonal structure in agreement with the earlier results of Jamieson, but the phase transition began at 80 + or - 5 kilobars, a somewhat lower value than generally reported. These experimental diffraction results are compared with the recent self-consistent pseudopotential calculations of Yin and Cohen (1981) and with the observed transition pressure for shock wave loaded Ge.

Baublitz, M., Jr.↗
NASA NTRS1978

Polymorphism and the crystal structures of InSb at elevated temperature and pressure

The paper presents polycrystalline X-ray diffraction data for three high-pressure phases of InSb. The study employed two types of diamond-anvil pressure cells. The X-ray diffraction parameters were recorded at different fixed pressures and temperatures on flat film. The experiment utilized Zr-filtered Mo radiation. The intensities were estimated from the X-ray photographs using a semiautomated microdensitometer.

Yu, S.-C.↗
NASA NTRS1982

Diffraction studies of the high pressure phases of GaAs and GaP

High pressure structural phase transitions of GaAs and GaP have been studied by energy dispersive X-ray diffraction with the radiation from the Cornell High Energy Synchrotron Source. GaAs began to transform at 172 + or - 7 kbar to an orthorhombic structure possibly belonging to space group Fmmm. GaP transformed to a tetragonal beta-Sn type phase at 215 + or - 8 kbar. Although pressure transmitting media were used to minimize shear stresses in the specimens, the high pressure diffraction results were interpreted as showing evidence for planar defects in the specimens.

Baublitz, M., Jr.↗
NASA NTRS1983

Pressure-induced phase transition of HgS

The high pressure phase transition of cinnabar (alpha-HgS) was studied by energy dispersive X-ray diffraction using a synchrotron X-ray source. The cinnabar crystal structure was found to transform to the sodium-chloride structure at about 130 kbar. The lattice parameter of the new phase was determined to be 5.070 + or - 0.005 A at 300 kbar. No further phase transition was observed up to 400 kbar.

Huang, T.↗
NASA NTRS1984

Ultrapressure materials science

Three active areas of research at ultra pressure are pursued, i.e., diffraction studies with the Cornell High Energy Synchrotron Source (CHESS), band gap and absorption edge effects, indentor-anvil experiments and theory and research to attain higher pressures. The range over which X-ray diffraction data and absorption edge data are obtained is extended to 700 kbars. Using the indentor technique pressures of 2.1 Mbars are obtained. Research results and methods are discussed.

Ruoff, A. L.↗
NASA NTRS1977

Consolidation of silicon nitride without additives

The feasibility of producing a sound, dense Si3N4 body without additives was explored, using conventional gas hot isostatic pressing techniques and an uncommon hydraulic hot isostatic pressing technique. These two techniques produce much higher pressure 275-413 MN/m sq (40,000 - 60,000 psi) than hot-pressing techniques. Evaluation was based on density measurement, microscopic examination, both optical and electron, and X-ray diffraction analysis. The results are summarized as follows: (1) Si3N4 can be densified to high density, greater than 95% of theoretical, without additions. (2) The higher density Si3N4 specimens appear to be associated with a greater amount of alpha to beta transformation. (3) Under high pressure, the alpha to beta transformation can occur at a temperature as low as 1150 C. (4) Grain deformation and subsequent recrystallization and grain refinement result from hot isostatic pressing of Si3N4.

Sikora, P. F.↗
NASA NTRS1984

Impact cratering: The process and its effects on planetary evolution

The potential for silicate-carbon dioxide reactions as a geochemical weathering agent on Venus was studied. A tholetitic basalt close to the composition determined by the XRF experiment at the Venera 14 sites was subjected to high temperature and pressure (with pure CO2 as the pressure medium) for varying time durations. The starting basalt material and the run products were examined optically and by X-ray diffraction and electron microscopy. The kinetics of the silicate-carbonate reactions is discussed. A study to elucidate details of impact processes and to assess the effects of impact cratering on planetary evolution is mentioned.

Grieve, R. A. F.↗
NASA NTRS1978

Stability of chromium (III) sulfate in atmospheres containing oxygen and sulfur

The stability of chromium sulfate in the temperature range from 880 K to 1040 K was determined by employing a dynamic gas-solid equilibration technique. The solid chromium sulfate was equilibrated in a gas stream of controlled SO3 potential. Thermogravimetric and differential thermal analyses were used to follow the decomposition of chromium sulfate. X-ray diffraction analysis indicated that the decomposition product was crystalline Cr2O3 and that the mutual solubility between Cr2(SO4)3 and Cr2O3 was negligible. Over the temperature range investigated, the decomposition pressure were significantly high so that chromium sulfate is not expected to form on commercial alloys containing chromium when exposed to gaseous environments containing oxygen and sulfur (such as those encountered in coal gasification).

Jacob, K. T.↗
NASA NTRS1982

Vaporization thermodynamics of K2S and K2SO3

The vaporization reactions, vapor pressures, and thermodynamics of potassium sulfide and potassium sulfite were studied for purposes of providing fundamental data for the seed cycle in magnetohydrodynamic electric power generation. Rate of effusion studies, supported by tube furnace experiments, X-ray powder diffraction, mass spectrometry and appropriate chemical analyses and tests, revealed that potassium sulfite disproportionates at high temperatures to form potassium sulfide and potassium sulfate. Potassium sulfide was observed to vaporize incongruently, the initial vapors beng predominantly potassium atoms, with minor species being S2 and various K-S molecules. The ratio of K/S2 in the vapor is very large initially and decreases steadily with prolonged heating. Several materials were evaluated for purposes of containing K2S/K2SO3 at temperatures or = 800 C: Pt, Mo, W, quartz, machinable glass, BN, high density graphite, pyrolytic coated graphite, and alumina. Of these, only alumina was observed to be chemically inert to both K2S but reacted with K2SO3. The other materials were not suitable for either substance. Thermodynamic calculations based on measured vapor pressures and approximate free energy functions are described. Results from isothermal total mass loss experiments and from thermogravimetric experiments are also included.

Bennet, J. E.↗
NASA NTRS1974

Single Crystal Membranes

Single crystal a- and c-axis tubes and ribbons of sodium beta-alumina and sodium magnesium beta-alumina were grown from sodium oxide rich melts. Additional experiments grew ribbon crystals containing sodium magnesium beta, beta double prime, beta triple prime, and beta quadruple prime. A high pressure crystal growth chamber, sodium oxide rich melts, and iridium for all surfaces in contact with the melt were combined with the edge-defined, film-fed growth technique to grow the single crystal beta-alumina tubes and ribbons. The crystals were characterized using metallographic and X-ray diffraction techniques, and wet chemical analysis was used to determine the sodium, magnesium, and aluminum content of the grown crystals.

Stormont, R. W.↗
NASA NTRS1983

Experiments with phase transitions at very high pressure

Diamond cells were constructed for use to 1 Mbar. A refrigerator for cooling diamond cells was adapted for studies between 15 and 300 K. A cryostat for superconductivity studies between 1.5 to 300 K was constructed. Optical equipment was constructed for fluorescence, transmission, and reflectance studies. X-ray equipment was adapted for use with diamond cells. Experimental techniques were developed for X-ray diffraction studies using synchrotron radiation. AC susceptibility techniques were developed for detecting superconducting transitions. The following materials were studied: compressed solidified gases (Xe, Ar), semiconductors (Ge, Si, GaAs), superconductors (Nb3Ge, Nb3Si, Nb3As, CuCl), molecular crystals (I).

Spain, I. L.↗
NASA NTRS1972

Silica reinforcement and char reactions in the Apollo heat shield.

Reactions of the silica reinforcement fiber and ablation char of the Apollo heat shield have been investigated by laboratory tests in an arc image furnace (at temperature levels up to 5000 R, pressures up to 0.7 atm, and heat flux similar to reentry) and by an actual reentry test. Microchemical analyses and X-ray diffraction studies have been made to determine the presence of SiC formation in the char. Experimental data and analytical predictions of thermal and density profiles have been compared for the ablation of virgin heat shield and precharred materials to determine the effects of SiC formation on ablation performance. In all analyses, general agreement was found between chemical composition and the thermal predictions for laboratory tests and reentry materials. In all ablated materials, SiC was formed in the front surface of the char. The highest SiC content found was 58% by weight and found in a high-pressure environment. The SiC formed was found to act as a heat sink in the ablation process and can lower the front surface temperature by 300 R.

Cagliostro, D. E.↗
NASA NTRS1984

High pressure cosmochemistry applied to major planetary interiors: Experimental studies

Progress is reported on a project to determine the properties and boundaries of high pressure phases of the H2-He-H2O-NH3-CH4 system that are needed to constrain theoretical models of the interiors of the major planets. This project is one of the first attempts to measure phase equilibria in binary fluid-solid systems in diamond anvil cells. Vibrational spectroscopy, direct visual observations, and X-ray diffraction crystallography of materials confined in externally heated cells are the primary experimental probes. Adiabats of these materials are also measured in order to constrain models of heat flow in these bodies and to detect phase transitions by thermal anomalies. Initial efforts involve the NH3-H2O binary. This system is especially relevant to models for surface reconstruction of the icy satellites of Jupiter and Saturn. Thermal analysis experiments were completed for the P-X space, p4GPa:0 or = 0.50, near room temperature. The cryostat, sample handling equipment, and optics needed to extend the optical P-T-X work below room temperature was completed.

Nicol, M. F.↗
NASA NTRS1972

Development of single crystal membranes

The design and construction of a high pressure crystal growth chamber was accomplished which would allow the growth of crystals under inert gas pressures of 2 MN/sq m (300 psi). A novel crystal growth technique called EFG was used to grow tubes and rods of the hollandite compounds, BaMgTi7O16, K2MgTi7O16, and tubes of sodium beta-alumina, sodium magnesium-alumina, and potassium beta-alumina. Rods and tubes grown are characterized using metallographic and X-ray diffraction techniques. The hollandite compounds are found to be two or three-phase, composed of coarse grained orientated crystallites. Single crystal c-axis tubes of sodium beta-alumina were grown from melts containing excess sodium oxide. Additional experiments demonstrated that crystals of magnesia doped beta-alumina and potassium beta-alumina also can be achieved by this EFG technique.

Stormont, R. W.↗
NASA NTRS1972

Hardness of kamacite and shock histories of 119 meteorites.

Use of metallographic and X-ray diffraction techniques to study the shock histories of 119 iron and stony-iron meteorites, and measurement of the hardness of kamacite in these specimens and in artificially shocked-unannealed and annealed meteorite specimens. Shock increases kamacite hardness, but complications introduced by other physical and chemical properties of meteorites limit its utility as a shock indicator. About 50% of the meteorites studied show evidence for preterrestrial shock loading to pressures of greater than or equal to 130 kb, and 40% have not been shocked to such high pressures. The remaining meteorites have been heat-altered in such a way that their shock histories cannot be determined explicitly. These results, together with those obtained previously, indicate that the plurality, if not the majority, of all iron and stony-iron meteorites sampled by the earth were shocked to pressures of greater than or equal to 130 kb during preterrestrial collisions between asteroidal-sized objects.

Jain, A. V.↗
NASA NTRS1979

Linear ruby scale and one megabar

The accuracy and validity of certain techniques used in studying high-pressure transitions have been investigated. Experiments which place upper limits of about 20 GPa and about 50 GPa on pressures practically attainable using uniaxial supported opposed anvil devices with tungsten carbide pistons and uniaxial opposed flat anvil diamond devices, respectively, are reported. Direct static determinations of the transition pressures of GaP by two different methods are described. The values obtained indicate that the linear ruby scale increasingly overestimates the transition pressure as the pressure rises above 10 GPa. It is further shown that the use of shock-based marker materials, such as silver, as the basis of pressure measurement in X-ray diffraction studies leads to bulk moduli of cubic carbides which are in extreme disagreement with expected values.

Ruoff, A. L.↗