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Results for “High pressure X-ray diffraction”

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All sourcesNASA NTRSDOE OSTI
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 NTRS1987

Heteroepitaxial growth of Cd(1-x)Mn(x)Te on GaAs by metalorganic chemical vapor deposition

In this letter, preliminary results are reported of heteroepitaxial growth of the dilute magnetic semiconductor alloy Cd(1-x)Mn(x)Te on GaAs by metalorganic chemical vapor deposition. Dimethylcadmium (DMCd), diethyltellurium (DETe), and tricarbonyl (methylcyclopentadienyl) manganese (TCPMn) were used as source materials. The TCPMn had to be heated to as high as 140 C to provide the required vapor pressure. Films with Mn atomic fractions up to 30 percent have been grown over the temperature range 410-450 C. Results of optical absorption/transmission, photoluminescence, and X-ray diffraction measurements are presented along with a scanning electron micrograph showing good surface morphology of the grown layers.

Nouhi, Akbar↗
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 NTRS1989

Mass spectrometric observations of metal oxychlorides produced by oxidation-chlorination reactions

It was recently reported that Cr2O3-forming alloys show less corrosion resistance than Al2O3-forming alloys in Cl2/O2 mixtures, which is attributed to the formation of porous Cr2O3 scales and stable CrO2Cl2 vapor species. This paper reports the results of direct mass spectrometric observations with a high-pressure sampling mass spectrometer of these metal oxychlorides forming on the surfaces of Hastelloy S and Alloy 600 superalloys. Samples were preoxidized for 2 hrs at 900 C before the exposure to a O2/Ar gas mixture containing 1 percent Cl2. Results of X-ray diffraction showed scales containing Cr2O3 and NiCr2O4 on both alloys. After exposure to Cl2, large quantities of Cr2O2Cl2 were demonstrated for both alloys, indicating that this is a route for the breakdown of Cr2O3 scales. The Mo present in the Hastelloy S leads to more rapid attack by Cl2, resulting in the formation of MoO2Cl2.

Jacobson, N. S.↗
NASA NTRS1988

Experimental study of planetary gases with applications to planetary interior models

High-pressure experimental data on planetary materials are critical in developing planetary models and in addressing otherwise insoluble problems of the internal structure of the major planets. Progress in the last five years has been particularly marked. Maximum static pressure of 550 GPa was achieved. For the first time, X-ray diffraction of solidified gases (Ne, Xe) and ices (H2O) were obtained at pressures above one megabar, single-crystal diffraction of ultralight elements (H2, He) were detected up to 25 GPa, pressures over 200 GPa at 77 K were reached in solid hydrogen, including the discovery of a phase transformation in the molecular solid. Advances in instrumentation and new measurements performed during 1983 to 1988 are summarized.

Bell, Peter M.↗
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 NTRS1991

Evaluation of a hydrogen resistant titanium aluminide alloy

The Ti-24Al-11Nb (Ti-24-11) alloy heat treated to the fine basketweave microstructure was shown previously to be hydrogen tolerant. In order to assess its limit of hydrogen tolerance, the tensile, creep, fracture toughness, and sustained load crack growth behaviors of this alloy were studied as a function of hydrogen content. All test specimens were thermally charged with internal hydrogen and tested at 25 and 600 C. Coupon specimens were used for developing the hydrogen charging procedures and for studying compatibility of the alloy with high temperature, high pressure gaseous hydrogen. The mechanical test results indicated that the fine basketweave microstructure was tolerant to hydride embrittlement for hydrogen contents up to approximately 1500 wt. ppm, providing that the hydride formed was of the TiH2 type. On the other hand, hydrogen charging experiments indicated that the Ti-24-11 alloy was severely cracked and pulverized under zero load when the hydrogen content exceeded 3000 wt. ppm. X-ray diffraction results revealed that the dichotomous behaviors might be due to the formation of TiH(1.924) type hydrides at higher hydrogen contents. Thus, hydrogen embrittlement in the Ti-24-11 alloy with the fine basketweave microstructure depends on hydrogen content and the nature of the hydrides formed.

Chan, K. S.↗
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 NTRS1990

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗
NASA NTRS1990

Lead-ruthenium pyrochlores as oxygen electrocatalysts

An investigation of lead-ruthenium pyrochlores of the structure Pb2(Ru/2-x/Pb/x/) O7-y for use as oxygen electrocatalysts in alkaline media is discussed. Lead-ruthenium pyrochlore mixed metal oxides were prepared and characterized by X-ray diffraction, BET surface area, dry powder conductivity, and chemical stability. Gas diffusion electrodes were developed specifically for the lead-ruthenium pyrochlore materials. Also investigated were the effects of varying electrode fabrication parameters on the oxygen reduction performance of the lead-ruthenium pyrochlore electrocatalyst. Long-term stability performance was also evaluated. The oxygen reduction performance of the pyrochlore electrocatalyst is considerably higher than that of the state-of-the-art gold-platinum alloy electrocatalyst currently used by NASA. Furthermore, the pyrochlore electrocatalysts are attractive candidates for high-performance pressurized alkaline fuel cells.

Anderson, E. B.↗
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.↗
NASA NTRS1981

Real-time observation of X-ray diffraction patterns with the Lixiscope

The feasibility of the Lixiscope (Low Intensity X-ray Imaging Scope) is demonstrated for real-time observation of transmission Laue patterns. Making use of the high-gain capability of microchannel plate (MCP) visible-light image intensifier tubes, X-ray images are converted to visible-light images by a scintillator. Pb discs are taped to the center of the Lixiscope input face, and crystal samples are held on a goniometer stage with modeling clay. With a compact size to facilitate off axis viewing, and real-time viewing to allow instantaneous response, the Lixiscope may prove useful in dynamic studies of the effects of plastic flows, stresses, high pressures, and low temperatures.

Chung, D. Y.↗
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↗