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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 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↗
NASA NTRS1986

X-ray investigations related to the shock history of the Shergotty achondrite

The shock stress suffered by naturally shocked materials from the Shergotty achondrite was studied using X-ray diffraction techniques and experimentally shocked augite and enstatite as standards. The Shergotty pyroxenes revealed the formation of continuous diffraction rings, line broadening, preferred orientation of small scale diffraction domains, and other evidence of substantial lattice disorders. As disclosed by the application of Debye-Scherrer techniques, they are hybrids between single crystals and fine-grained random powders. The pyroxene lattice is very resistant to shock damage on smaller scales. While measurable lattice disaggregation and progressive fragmentation occur below 25 GPa, little additional damage is suffered from application of pressures between 30 to 60 GPa, making pressure calibration of naturally shocked pyroxenes via X-ray methods difficult. Powder diffractometer scans on pure maskelynite fractions of Shergotty revealed small amounts of still coherently diffracting plagioclase, which may contribute to the high refractive indices of the diaplectic feldspar glasses of Shergotty.

Horz, F.↗
NASA NTRS1981

The effect of mechanical surface and heat treatments on the erosion resistance of 6061 aluminum alloy

The effects of both mechanical surface treatments and heat treatments on the erosion resistance of 6061 aluminum alloy were studied in order to gain a better understanding of material properties which affect erosion behavior. It was found that mechanical surface treatments have little or no effect on the erosion resistance. This is due to the formation by particle impact of a work-hardened surface layer, independent of the initial surface condition. The erosion resistance of aluminum single crystals was found to be independent of orientation, which is due to destruction of the surface microstructure and formation of a polycrystalline surface layer by the particle impact as observed by X-ray diffraction. Although on solution treatment of annealed aluminum 6061 the increase in hardness is accompanied by an increase in erosion resistance, precipitation treatment (which causes a further increase in hardness) results in a slightly lower erosion resistance.

Salik, J.↗
NASA NTRS1980

Effect of mechanical surface and heat treatments on erosion resistance

The effects of mechanical surface treatments as well as heat treatments on the erosion resistance of 6061 aluminum alloy and 1045 steel were studied. Mechanical surface treatments were found to have little or no effect on the erosion resistance. This is due to the formation by particle impact of a work hardened surface layer regardless of the initial surface condition. The erosion resistance of Al single crystals is found to be independent of orientation. This is due to destruction of the surface microstructure and formation of a polycrystalline surface layer by the impact of erodant particles as observed by X-ray diffraction. While upon solution treatment of annealed 6061 aluminum the increase in hardness is accompanied by an increase in erosion resistance, precipitation treatment which causes a further increase in hardness results in slightly lower erosion resistance. Using two types of erodant particles, glass beads and crushed glass, the erosion rate is found to be strongly dependent on erodant particle shape, being an order of magnitude higher for erosion with crushed glass as compared to glass beads. While for erosion with glass beads heat treatment of 1045 steel had a profound effect on its erosion resistance, little or no such effect was observed for erosion with crushed glass.

Salik, J.↗
NASA NTRS1985

Temperature dependence of gamma-gamma prime lattice mismatch in nickel-base superalloys

High temperature X-ray diffraction techniques were used to determine the gamma-gamma prime lattice mismatch of three different nickel-base superalloys at temperatures between 18 and 1000 C. The measurements were performed on oriented single-crystal disks which had been aged to produce a semicoherent gamma-gamma prime structure. The thermal expansion of the lattice parameters of the gamma and gamma-prime phases was described by a second-order polynomial expression. The expansion of the gamma-prime phase was consistently smaller than that of the gamma phase, which caused the lattice mismatch to become more negative at higher temperatures. It was also shown that high values of lattice mismatch resulted in increased rates of directional gamma-prime coarsening during elevated temperature creep exposure.

Nathal, M. V.↗
NASA NTRS1982

Influence of cobalt, tantalum, and tungsten on the microstructure and mechanical properties of superalloy single crystals

The influence of Co, Ta, and W on the microstructure and mechanical properties of nickel base super-alloy single crystals was investigated. A matrix of alloys was based on Mar-M 247 stripped of C, B, Zr, and Hf. The microstructures of the alloys were examined using optical and electron microscopy, phase extraction, X-ray diffraction, and differential thermal analysis. Tensile and creep-rupture tests were performed at 1000 C. An increase in tensile and creep strength resulted when Co was removed from alloys containing high refractory metal contents, but Co effects were negligible for alloys with lower refractory metal levels. In the composition range studied, W was more effective than Ta in increasing the creep resistance. The mechanical properties are discussed in relation to the microstructures of the alloys.

Nathal, M. V.↗
NASA NTRS1982

Study of the photovoltaic effect in thin film barium titanate

Ferroelectric films of barium titanate were synthesized on silicon and quartz substrates, and the photoelectric effect in the structure consisting of metal deposited ferroelectric barium titanate film silicon was studied. A photovoltage with polarity that depends on the direction of the remanent polarization was observed. The deposition of BaTiO3 on silicon and fused quartz substrates was accomplished by an rf sputtering technique. A series of experiments to study the growth of ferroelectric BaTiO3 films on single crystal silicon and fused quartz substrates were conducted. The ferroelectric character in these films was found on the basis of evidence from the polarization electric field hysteresis loops, capacitance voltage and capacitance temperature techniques and from X-ray diffraction studies.

Grannemann, W. W.↗
NASA NTRS1974

Spectrometric properties of crystals for X-ray astronomy. I

Preliminary results are reported on measurements of X-ray reflection coefficients, rocking-curve width estimates, and factors that influence these for KAP, EDDT, and ADP crystals. The agreement between parameters measured in the authors' laboratory and others over a period of some ten years, and the uniformity among the authors' samples, indicate that KAP as commercially supplied is amenable to a single theoretical description. This permits application of X-ray diffraction theory, which outlined and compared to measurements with good agreement.

Burek, A. J.↗
NASA NTRS1979

X-ray diffraction studies of shocked lunar analogs

The X-ray diffraction experiments on shocked rock and mineral analogs of particular significance to lunar geology are described. Materials naturally shocked by meteorite impact, nuclear-shocked, or artificially shocked in a flat plate accelerator were utilized. Four areas were outlined for investigation: powder diffractometer studies of shocked single crystal silicate minerals (quartz, orthoclase, oligoclase, pyroxene), powder diffractometer studies of shocked polycrystalline monomineralic samples (dunite), Debye-Scherrer studies of single grains of shocked granodiorite, and powder diffractometer studies of shocked whole rock samples. Quantitative interpretation of peak shock pressures experienced by materials found in lunar or terrestrial impact structures is presented.

Hanss, R. E.↗
NASA NTRS1974

Fluid flow effects on crystalline perfection

Optimum solidification parameters for the production of highly perfect copper crystals by Czochralski growth are sought along with the documentation of crystal imperfections under various growth conditions. X-ray techniques which do not in their application produce defects and which allow the characterization of imperfections in single crystals are chosen to assess crystal perfection. The X-ray techniques employed ranged from ordinary Laue photography through Borrmann topography to double-crystal scanning diffractometry, thus allowing crystals with a wide variation in perfection to be studied. As a set of controllable solidification parameters, the rotation of the seed and of the melt and the diameter of the bottleneck are chosen. X-ray diffraction topographs are analyzed along with the data obtained from rocking curve measurements. Tables of growth conditions and quantitative data of rocking curve widths are presented.

Kuriyama, M.↗
NASA NTRS1981

Silicide surface phases on gold

The crystalline silicide layers formed on (111) and (100) surfaces of Au films on various Si single-crystal substrates are studied by LEED and AES in conjunction with sputter-depth profiling as a function of annealing temperature. On the (111) surface, three basic silicide structures are obtained corresponding to layers of various thicknesses as obtained by different preparation conditions. The (100) surface shows only two different structures. None of the structures is compatible with the various bulk silicide structures deduced from X-ray diffraction. Using LEED as a criterion for the presence or absence of silicide on the surface, smaller layer thicknesses are obtained than reported previously on the basis of AES studies.

Green, A. K.↗
NASA NTRS1975

Evaluation of silicon ribbon material for solar cell fabrication

Optical microscopy, electron microscopy, and X-ray diffraction were utilized to characterize silicon ribbon structure. Complex twin formation was observed in nearly all ribbons examined. Twins formed in the 110-plane 112-line ribbon orientation appear stable, and this orientation may be preferable when the ribbon is utilized for solar cells. In addition to twinning, grain boundaries and other structural defects were observed in the ribbon material. Hall effect, resistivity, spreading resistance, surface photovoltage, and solar cell electrical/optical measurements were performed on ribbon samples and correlated with structural and ribbon growth characteristics. Only those ribbon samples with either single-crystal structure or with 'parallel' twin formations were capable of solar-cell performance approaching that of Czochralski material.

Leipold, M.↗
NASA NTRS1976

Interaction of metal layers with polycrystalline Si

Solid-phase reactions of metal films deposited on 0.5-micron-thick polycrystalline layers of Si grown by chemical vapor deposition at 640 C were investigated by MeV He-4 backscattering spectrometry, glancing angle X-ray diffraction, and SEM observations. For the metals Al, Ag, and Au, which form simple eutectics, heat treatment at temperatures below the eutectic results in erosion of the poly-Si layer and growth of Si crystallites in the metal film. Crystallite formation is observed at temperatures exceeding 550 C for Ag, at those exceeding 400 C for Al, and at those exceeding 200 C for Au films. For Pd, Ni, and Cr, heat treatment results in silicide formation. The same initial silicides (Pd2Si, Ni2Si, and CrSi2), are formed at similar temperatures on single-crystal substrates.

Nakamura, K.↗
NASA NTRS1986

Growth of high-quality thin-film Ge single crystals by plasma-enhanced chemical vapor deposition

Thin-film Ge single crystals (approx. 10 microns) have been epitaxially grown on polished NaCl(100) substrates at 450C by using plasma-enhanced chemical vapor deposition. Films on approximately 1 sq cm and larger were separated from the NaCl by either melting the salt or by differential shear stress upon cooling to room temperature. The ordered growth of the Ge was found to be most sensitive to the initial plasma power and to the continuum flow dynamics within the carbon susceptor. The films were visually specular and exhibited a high degree of crysalline order when examined by X-ray diffraction. The films were found to be p-type with a carrier concentration of approximately 3 x 10 to the 16th power/cu cm, a resistivity of 0.11 ohm-cm, and a Hall hole mobility of 1820 sq cm/v/s at room temperature. Vacuum firing minimized the primary contaminant, Na, and corresponding lowered the carrier concentration to 4 x 10 to the 14th power/cu cm.

Outlaw, R. A.↗
NASA NTRS1978

A microstructural study of the Tishomingo meteorite

Metallography, electron microscopy, and X-ray diffraction techniques were employed to study a fragment of the Tishomingo iron meteorite. The results suggest the following thermal-mechanical history: The fragment was originally a large crystal of taenite (gamma). Cooling through the alpha + gamma phase boundary did not result in accompanying precipitation of kamacite (alpha). Transformation to a martensitic structure initiated between -25 and -65 C. Transformation continued as the temperature fell to -75 to -115 C, resulting in approx 80% martensite (alpha-prime). Subsequent shock deformation and thermal aging processes substantially modified the taenite and martensite microstructures. Twins in the retained taenite phase are attributed to shock deformation at a pressure estimated for a single event at about 170 kbar. The existing complex altered martensite structure containing both taenite and kamacite (3-15% Ni) particles was apparently the product of both shock deformation and thermal aging processes. The maximum temperature reached during thermal aging is estimated to be less than 400 C and perhaps below 310 C.

Ives, L. K.↗
NASA NTRS1984

Free-standing thin film Ge single crystals grown by plasma-enhanced chemical vapor deposition

The films, which are approximately 10 microns in thickness, are grown epitaxially on polished (100) NaCl substrates at 450 C by plasma enhanced chemical vapor deposition. Upon cooling, the films are separated from the substrate by differential shear stress, leaving free-standing films of Ge which can be handled. Growths are attained by nucleating at minimum plasma power for very brief intervals and then raising the power to 65 W to increase the growth rate to approximately 10 microns/h. It is found that substrate exposure to the plasma at too high a power for too long a time sputters and erodes the surface, thereby substantially degrading the nucleation process and the ultimate growths. It is noted that the free-standing films are visually specular and exhibit a high degree of crystalline order when examined by X-ray diffraction. Auger electron spectroscopy and energy dispersive analysis of X-rays reveal no detectable bulk contamination.

Outlaw, R. A.↗
NASA NTRS1966

X-ray analysis of fatigue damage in copper

A Warren-Averbach x-ray line profile analysis was applied to, broadened x-ray diffraction peaks from copper deformed in fatigue. The copper specimens were fatigued by four point bending at various strain amplitudes, and measurements were made at various fractions of the total fatigue life. The analysis results in an estimation of 1) an average coherently diffracting domain size in a direction normal to the diffracting planes; and 2) a strain distribution function. The strain distribution function is in terms of the root mean square strain, <ϵ^(2)> where ϵ is averaged over a given distance at all points in the diffracting crystals. This rms strain is expressed as a function of averaging distance for a direction normal to the diffracting planes. The rms strains were found to be a function of the fatigue strain amplitude level, increasing with amplitude and reaching a maximum limiting value during the first 2% of the fatigue life. The strains were normally larger in the 4lO0 direction compared to the <111> direction and the absolute values were quite small. These results may be explained by assuming the dislocations are present in the form of dipoles because the lattice strain around a dipole is much less than around single dislocations. Conclusions arrived at in this analysis are in agreement with current theories of fatigue damage in metals. The result that maximum hardening is achieved during the initial few percent of the fatigue life is confirmed by many other investigators using entirely different analytical techniques. It is felt that the structure of the material is changing during this initial hardening stage to an eventual steady state characteristic of the testing conditions. A unique substructure is developed which thereafter persists, and the remainder of the fatigue test is taken up by crack propagation through this substructure until ultimate failure occurs by fracture. The formation of this steady state structure is dependent on the maximum fatigue strain amplitude and on the frequency and temperature of cycling for a particular material.

COPPER↗