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NASA NTRS1989

Superconducting ceramics in the Bi1.5SrCaCu2O sub x system by melt quenching technique

Bi sub 1.5 SrCaCu sub 2 O sub x has been prepared in the glassy state by rapid quenching of the melt. The kinetics of crystallization of various phases in the glass have been evaluated by a variable heating rate differential scanning calorimetry method. The formation various phases on thermal treatments of the glass has been investigated by powder X-ray diffraction and electrical resistivity measurements. Heating at 450 C formed Bi sub 2 Sr sub 2 CuO sub 6, which disappeared on further heating at 765 C, where Bi sub 2 Sr sub 2 CaCu sub 2 O sub 8 formed. Prolonged heating at 845 C resulted in the formation of a small amount of a phase with T sub c onset of approx. 108 K, believed to be Bi sub 2 Sr sub 2 Ca sub 2 Cu sub 3 O sub 10. This specimen showed zero resistivity at 54 K. The glass ceramic approach could offer several advantages in the fabrication of the high-T sub c superconductors in desired practical shapes such as continuous fibers, wires, tapes, etc.

Bansal, Narottam P.↗

NASA NTRS1990

Polysiloxanes derived from the controlled hydrolysis of tetraethoxysilane as precursors to silica for use in ceramic processing

Synthesis, properties, and potential applications in ceramic processing for two polysiloxane silica precursors derived from the controlled hydrolysis of tetraethoxysilane (TEOS) are presented. The higher molecular weight TEOS-A is a thick adhesive liquid of viscosity 8000 to 12,000 c.p. having a SiO2 char yield of about 55 percent. The lower molecular weight TEOS-B is a more fluid liquid of viscosity 150 to 200 c.p. having a SiO2 char yield of about 52 percent. The acid catalyzed hydrolysis of TEOS to hydrated silica gel goes through a series of polysiloxane intermediates. The rate of this transition increases with the quantity of water added to the TEOS; thus, for ease of polymer isolation, the amount of water added must be carefully determined so as to produce the desired polymer in a reasonable time. The water to TEOS mole ratio falls in the narrow range of 1.05 for TEOS-A and 0.99 for TEOS-B. Further polymerization or gelation is prevented by storing at -5 C in a freezer. Both polysiloxanes thermoset to a glassy solid at 115 C. The liquid polymers are organic in nature in that they are miscible with toluene and ethanol, slightly souble in heptane, but immiscible with water. For both polymers, results on viscosity versus time are given at several temperatures and water additions. Based on these results, some examples of practical utilization of the precursors for ceramic fabrication are given.

Philipp, Warren H.↗

NASA NTRS1990

Optical constants of solid methane

Methane is the most abundant simple organic molecule in the outer solar system bodies. In addition to being a gaseous constituent of the atmospheres of the Jovian planets and Titan, it is present in the solid form as a constituent of icy surfaces such as those of Triton and Pluto, and as cloud condensate in the atmospheres of Titan, Uranus, and Neptune. It is expected in the liquid form as a constituent of the ocean of Titan. Cometary ices also contain solid methane. The optical constants for both solid and liquid phases of CH4 for a wide temperature range are needed for radiative transfer calculations, for studies of reflection from surfaces, and for modeling of emission in the far infrared and microwave regions. The astronomically important visual to near infrared measurements of solid methane optical constants are conspicuously absent from the literature. Preliminary results are presented on the optical constants of solid methane for the 0.4 to 2.6 micrometer region. Deposition onto a substrate at 10 K produces glassy (semi-amorphous) material. Annealing this material at approximately 33 K for approximately 1 hour results in a crystalline material as seen by sharper, more structured bands and negligible background extinction due to scattering. The constant k is reported for both the amorphous and the crystalline (annealed) states. Typical values (at absorption maxima) are in the .001 to .0001 range. Below lambda = 1.1 micrometers the bands are too weak to be detected by transmission through the films less than or equal to 215 micrometers in thickness, employed in the studies to date. Using previously measured values of the real part of the refractive index, n, of liquid methane at 110 K, n is computed for solid methane using the Lorentz-Lorenz relationship. Work is in progress to extend the measurements of optical constants n and k for liquid and solid to both shorter and longer wavelengths, eventually providing a complete optical constants database for condensed CH4.

Khare, Bishun N.↗

NASA NTRS1990

Survival of carbon grains in shocks

Supernova shocks play a significant part in the life of an interstellar grain. In a typical 10 to the 9th power year lifetime, a grain will be hit by an average of 10 shocks of 100 km s(sup -1) or greater velocity, and even more shocks of lower velocity. Evaluation of the results of this frequent shock processing is complicated by a number of uncertainties, but seems to give about 10 percent destruction of silicate grains and about half that for graphite grains. Because of the frequency of shocking, the mineralogy and sizes of the grain population is predominately determined by shock processing effects, and not by the initial grain nucleation and growth environment. One consequence of the significant role played by interstellar shocks is that a certain fraction (up to 5 percent) of the carbon should be transformed into the diamond phase. Diamond transformation is observed in the laboratory at threshold shock pressures easily obtainable in grain-grain collisions in supernova shocks. Yields for transforming graphite, amorphous carbon, glassy carbon, and other nearly pure carbon solids into diamond are quite high. Impurities up to at least the 10 percent level (for oxygen) are tolerated in the process. The typical size diamond expected from shock transformation agrees well with the observed sizes in the Lewis et al. findings in meteoritic material. Isotropic anomalies already contained in the grain are likely to be retained through the conversion process, while others may be implanted by the shock if the grain is close to the supernova. The meteoritic diamonds are likely to be the results of transformation of carbon grains in grain-grain collisions in supernova shock waves.

Seab, C. Gregory↗

NASA NTRS1990

Aerobraking in a dusty Martian atmosphere

The effects of dust particle impacts on the erosion of the heat shield were estimated for a 26 m diameter aerobraking vehicle entering the Mars atmosphere at 8.6 km/sec. An explicit Navier-Stokes code was used to compute the flow field about the vehicle for the actual Martian atmospheric composition at a speed of 7.5 km/sec. The deceleration and melting of the dust particles within the forebody shock-layer was computed for dust spherules having initial diameters from 3 to 10 microns. Two heat shield materials were considered: Shuttle tiles with glassy surfaces and a low-density ablator known as Avcoat.

Chang, I-Dee↗

NASA NTRS1990

Petrology and mineralogy of Type II, FeO-rich chondrules in Semarkona (LL3.0) - Origin by closed-system fractional crystallization, with evidence for supercooling

The petrology of type II porphyritic olivine chondrules in Semarkona (LL3.0) has been studied in detail. Olivines in these chondrules are euhedral, Fe-rich, and are strongly zoned from cores to rims of grains in FeO (Fa10-30), Cr2O3 (0.2-0.6 wt pct), MnO (0.2-0.7 wt pct), and CaO (0.1-0.4 wt pct). Interstitial mesostasis is rich in Si, Al, and Ca and is glassy with abundant microcrystallites. Minor minerals include troilite, Fe,Ni metal, and chromite. Some olivine grains contain euhedral, fayalite-rich cores that are probably produced during initial supercooling of the chondrule melt. Rare relict grains of forsteritic olivine have compositions very similar to olivines in type IA chondrules in Semarkona and may result from disaggregation of such chondrules. Apart from these relics, all properties of type II chondrules can be described by closed-system fractional crystallization of droplets which were essentially entirely molten. Type IA chondrules may have formed from type II chondrules by loss of Fe and volatiles. Alternatively, the two chondrule types may have formed in regions of considerable diversity in the solar nebula from precursor materials with different Fe/Mg ratios.

Jones, Rhian H.↗

NASA NTRS1990

Superconducting Bi(1.5)Pb(0.5)Sr2Ca2Cu3O(x) ceramics by rapid melt quenching and glass crystallization

The preparation of superconducting Bi(1.5)Pb(0.5)Sr2Ca2Cu3O(x) in the glassy state is described, and the results of a study of its crystallization kinetics are presented. The annealing parameters for transforming the glass into a superconductor containing a large fraction of the high-Tc phase were determined. It was found that prolonged annealing (longer than 10 days) in air at 840 C, followed by slow cooling, results in the Tc of 107.2 K and a sharp transition of 2 K.

Bansal, Narottam P.↗

NASA NTRS1991

Electrochemical Deposition Of Conductive Copolymers

Experiments show electrically conductive films are deposited on glassy carbon or indium tin oxide substrates by electrochemical polymerization of N-{(3-trimethoxy silyl) propyl} pyrrole or copolymerization with pyrrole. Copolymers of monomer I and pyrrole exhibit desired electrical conductivity as well as desired adhesion and other mechanical properties. When fully developed, new copolymerization process useful in making surface films of selectable conductivity.

Nagasubramanian, Ganesan↗

NASA NTRS1989

Steps toward interstellar silicate dust mineralogy

One of the most certain facts on interstellar dust is that it contains grains with silicon oxygen tetrahedra (SOT), the internal vibrations of which cause the well known silicate bands at 10 and 18 microns. The broad and almost structureless appearance of them demonstrates lack of translation symmetry in these solids that must be considered amorphous or glassy silicates. There is no direct information on the cations in these interstellar silicates and on the number of bridging oxygens per tetrahedron (NBO). Comparing experimental results gained on amorphous silicates, e.g., silicate glasses, of cosmically most abundant metals (Mg, Fe, Ca, Al) with the observations is the only way to investigate interstellar silicate dust mineralogy (cf, Dorschner and Henning, 1986). At Jena University Observatory IR spectra of submicrometer-sized grains of pyroxene glasses (SSG) were studied. Pyroxenes are common minerals in asteroids, meteorites, interplanetary, and supposedly also cometary dust particles. Pyroxenes consist of linearly connected SOT (NBO=2). In the vitreous state reached by quenching melted minerals, the SOT remain nearly undistorted (Si-O bond length unchanged); the Si-O-Si angles at the bridging oxygens of pyroxenes, however, scatter statistically. Therefore, the original cation oxygen symmetry of the crystal (octahedral and hexahedral coordination by O) is completely lost. The blended bands at 10 and 18 microns lose their diagnostic differences and become broad and structureless. This illustrates best the basic problem of interstellar silicate mineral diagnostics. Optical data of glasses of enstatite, bronzite, hypersthene, diopside, salite, and hedenbergite have been derived. Results of enstatite (E), bronzite (B), and hypersthene (H) show very good agreement with the observed silicate features in the IR spectra of evolutionarily young objects that show P-type silicate signature according to the classification by Gurtler and Henning (1986). Compositional parameters and main characteristics of experimental SSG spectra in IR for the glasses E, B, and H are shown in tabular form. Results fit excellently the relations derived by Koike and Hasegawa (1987) and suggest that the band ratio of the astronomical silicate by Draine and Lee (1984) is too low.

Dorschner, J.↗

NASA NTRS1991

Comparison of dynamic fatigue behavior between SiC whisker-reinforced composite and monolithic silicon nitrides

The dynamic fatigue behavior of 30 vol percent silicon nitride whisker-reinforced composite and monolithic silicon nitrides were determined as a function of temperature from 1100 to 1300 C in ambient air. The fatigue susceptibility parameter, n, decreased from 88.1 to 20.1 for the composite material, and from 50.8 to 40.4 for the monolithic, with increasing temperature from 1100 to 1300 C. A transition in the dynamic fatigue curve occurred for the composite material at a low stressing rate of 2 MPa/min at 1300 C, resulting in a very low value of n equals 5.8. Fractographic analysis showed that glassy phases in the slow crack growth region were more pronounced in the composite compared to the monolithic material, implying that SiC whisker addition promotes the formation of glass rich phases at the grain boundaries, thereby enhancing fatigue. These results indicate that SiC whisker addition to Si3 N4 matrix substantially deteriorates fatigue resistance inherent to the matrix base material for this selected material system.

Choi, Sung R.↗

NASA NTRS1991

Glass formation and crystallization in high-temperature glass-ceramics and Si3N4

The softening of glassy grain boundaries in ceramic matrix composites and Si3N4 at high temperatures reduces mechanical strength and the upper-use temperature. By crystallizing this glass to a more refractory crystalline phase, a material which performs at higher temperatures may result. Three systems were examined: a cordierite composition with ZrO2 as a nucleating agent; celsian compositions; and yttrium silicate glasses both in bulk and intergranular in Si3N4. For the cordierite compositions, a series of metastable phases was obtained. The crystallization of these compositions was summarized in terms of metastable ternary isothermal sections. Zircon formed at the expense of ZrO2 and spinel. In SiC composites, the transformations were slower. In celsian, two polymorphs were crystallized. One phase, hexacelsian, which always crystallized, even when metastable, had an undesirable volume change. The other phase, celsian, was very difficult to crystallize. In yttrium silicate bulk glasses, similar in composition to the intergranular glass in Si3N4, a number of polymorphs of Y2Si2O7 were crystallized. The conditions under which these polymorphs formed are compared with crystallization in Si3N4.

Drummond, Charles H., III↗

NASA NTRS1989

Mineralogical and chemical properties of the lunar regolith

The composition of lunar regolith and its attendant properties are discussed. Tables are provided listing lunar minerals, the abundance of plagioclase feldspar, pyroxene, olivine, and ilmenite in lunar materials, typical compositions of common lunar minerals, and cumulative grain-size distribution for a large number of lunar soils. Also provided are charts on the chemistry of breccias, the chemistry of lunar glass, and the comparative chemistry of surface soils for the Apollo sites. Lunar agglutinates, constructional particles made of lithic, mineral, and glass fragments welded together by a glassy matrix containing extremely fine-grained metallic iron and formed by micrometeoric impacts at the lunar surface, are discussed. Crystalline, igneous rock fragments, breccias, and lunar glass are examined. Volatiles implanted in lunar materials and regolith maturity are also addressed.

Mckay, David S.↗

NASA NTRS1990

Influence of several metal ions on the gelation activation energy of silicon tetraethoxide

The effects of nine metal cations Li(+), Na(+), Mg(2+), Ca(2+), Sr(2+), Cu(2+), Al(3+), La(3+), and Y(3+) on silica gel formation has been investigated by studying the hydrolysis and polycondensation of silicon tetraethoxide (TEOS) in the presence of metal nitrates. The influence of water:TEOS mole ratio, metal ion concentration, and the reaction temperature has been investigated. The overall activation energy for gel formation has been determined from the temperature dependence of the time of gelation for each system. The activation energy for -Si-O-Si- network formation is found to be 54.5 kJ/mol. The gel formation time as well as the activation energy sharply increase in the presence of Cu(2+), Al(3+), La(3+) and Y(3+). In contrast, the presence of Li(+), Na(+), Mg(2+), Ca(2+), or Sr(2+) lowers the gelation time, but has no appreciable effect on the activation energy. This difference may be attributed to the participation or nonparticipation of the metal ions in the formation of the three-dimensional polymeric network during the polycondensation step. The concentration of metal ion Mg(2+), Ca(2+), Y(3+) or the water:TEOS mole ratio had no appreaciable effect on the gelation activation energy. A simple test has been proposed to determine whether a metal ion would act as a network intermediate or modifier in silica and other glassy networks.

Bansal, Narottam P.↗

NASA NTRS1990

Effect of high temperature hydrogen exposure on the strength and microstructure of mullite

The corrosion of near stoichiometric mullite (3Al2O3-2SiO2) by pure dry hydrogen gas was studied at 1050 and 1250 C for times up to 500 hr. The hydrogen preferentially attacked the grain boundaries of the mullite where an aluminosilicate glass was present. Corrosion of the mullite grains was observed after 125 hr at 1250 C. The hydrogen reaction removed SiO2 from the glassy grain boundaries and the mullite grains resulting in a porous alumina rich surface. At 1250 C the strength increased after short exposure times (at least up to 125 hr) and decreased by 53 percent after 500 hr. At 1050 C, all exposure times (25 to 500 hr) decreased the strength. At 500 hr room temperature strength of mullite exposed to 1050 C was reduced by 22 percent. The strength reduction after short exposure times at 1050 C is attributed to crystallization of the grain boundary glass phase.

Herbell, Thomas P.↗

NASA NTRS1990

Formation conditions of pyroxene-olivine and magnesian olivine chondrules

Dynamic crystallization experiments performed on a Type I and an intermediate Type II/III composition demonstrate chondrule texture is controlled by the abundance of heterogeneous nuclei. This factor is controlled by the maximum initial temperature relative to the olivine disappearance temperature for the given heating time. Glassy and excentroradial textures form from superheated melts with no nuclei, and barred textures form with initial temperatures near the olivine disappearance temperature. Porphyritic and granular textures form with initial temperatures below the liquidus with abundant nuclei. Comparison of zoning characteristics of experimental olivines with those in natural porphyritic olivine chondrules indicates cooling rates of 100 to 1000 C/h, whereas olivine morphology indicates barred olivines cooled at rates of 250 to 1000 C/h. Texture/composition relationships suggest chondrules experienced initial temperatures below 1750 C. These observations are consistent with the idea that chondrules formed by transient heating in dust-rich regions (i.e., in the midplane) of the solar nebula.

Radomsky, Patrick M.↗

NASA NTRS1991

Phase transformations and the spectral reflectance of solid sulfur - Can metastable sulfur allotropes exist on Io?

Laboratory investigations have been conducted on the effects of variations in sulfur sample histories on their solid-state transformation rate and the corresponding spectral variation of freshly frozen sulfur. The temporal variations in question may be due to differences in the amount and type of metastable allotropes present in the sulfur after solidification, as well as to the physics of the phase-transformation process itself. The results obtained are pertinent to the physical behavior and spectral variation of such freshly solidified sulfur as may exist on the Jupiter moon Io; this would initially solidify into a glassy solid or monoclinic crystalline lattice, then approach ambient dayside temperatures. Laboratory results imply that the monoclinic or polymeric allotropes can in these circumstances be maintained, and will take years to convert to the stable orthorhombic crystalline form.

Moses, Julianne I.↗

NASA NTRS1991

Silsesquioxane-derived ceramic fibres

Fibers formed from blends of silsesquioxane polymers were characterized to study the pyrolytic conversion of these precursors to ceramics. The morphology of fibers pyrolyzed to 1400 C revealed primarily amorphous glasses whose conversion to beta-SiC is a function of both blend composition and pyrolysis conditions. Formation of beta-SiC crystallites within the glassy phase is favored by higher than stoichiometric C/Si ratios, while carbothermal reduction of Si-O bonds to form SiC with loss of SiO and CO occurs at higher methyl/phenylpropyl silsesquioxane (lower C/Si) ratios. As the carbothermal reduction is assumed to be diffusion controlled, the fibers can serve as model systems to gain understanding of the silsesquioxane pyrolysis behavior, and therefore are useful in the development of polysilsesquioxane-derived ceramic matrices and coatings as well.

Hurwitz, F. I.↗

NASA NTRS1991

Why are blue zhamanshinites blue? Liquid immiscibility in an impact melt

A study of the cause of the coloration of blue zhamanshinites, which are glassy impact melt rocks from the Zhamanshin crater in the USSR are reported. It is found that the blue color results from Rayleigh scattering from spherical, 100 nm-diameter inclusions of a separate Ca-Fe-Mg-P-rich silicate glass. These observations can best be explained by the operation of liquid immiscibility in the zhamanshinite melt, and suggest that liquid immiscibility may have a more general role in impactite evolution.

Zolensky, Michael E.↗