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At least 145 records · Page 8

Nature and origin of mineral coatings on volcanic rocks of the Black Mountain, Stonewall Mountain and Kane Springs wash volcanic centers, southern Nevada

Mineral coatings, including desert varnish on volcanic rocks of the semi-arid Basin and Range province are composted of amorphous, translucent films of Fe, Mn, Si, and Al rich compounds. Coatings are chiefly thin films that impregnate intergranularly to depths of about 0.1 to 0.3 mm, rarely deeper. Sixteen coating sections and subsurface interiors were probed by SEM; 20 samples were scanned by infrated spectrometry; 10 samples were scanned for visible-near IR spectra; inductin coupling plasma analyses were collected on 34 samples; 2 desert varnish surgaces were investigated by optical density slice imagery; a few XRD analyses were conducted in addition to the 50 reported in the last period; thin section observation continued; and imagery processing focused on classification techniques. In late May, approximately 10 field days were spent at the Stonewall and Black Mountain study sited conducting more detailed mapping and observation base on imagery results and collecting spectra with the Collins Field Spectrometer. Approximately 100 spectral analyses were collected and are currently being processed.

Taranik, James V.↗

High-temperature oxidation of a rapidly solidified amorphous Ta-Ir alloy

The oxidation products formed at 500 and 700 C on an amorphous Ta-44.5 at. pct Ir alloy in an Ar-0.1 percent O2 gas mixture were characterized using SEM, XRD, EPMA, TEM, STEM, AES, and XPS. Initially, a thin (3-4 nm) layer of Ta2O5 formed at the surface of the alloy. Continued growth of the Ta2O5, which occurred very rapidly, involved diffusion of oxygen anions from the Ta2O5/gas interface to the alloy/Ta2O5 interface, where tantalum was selectively oxidized. Because the oxide grew more quickly than iridium could diffuse back into the alloy, the iridium coalesced into platelets of crystalline iridium-rich alloy that were oriented approximately parallel to the oxide/alloy interface, and which became embedded in a matrix of Ta2O5. The unoxidized core remained in the glassy state. The oxidation process and/or the dissolution of oxygen into the unoxidized alloy caused the alloy to become embrittled.

Cotell, Catherine M.↗

Phase purity of NiCo2O4, a catalyst candidate for electrolysis of water

NiCo2O4 is shown to be difficult to obtain as a pure phase, and may never have been so obtained. High resolution x-ray diffractometry is required for its precise characterization. Film XRD is not likely to show the asymmetry in the spinel diffraction lines, caused by poorly crystallized NiO, as seen in diffractometer traces. The Co3O4 which is expected to accompany NiO as an impurity in NiCo2O4 syntheses has the same diffraction pattern as the binary oxide. Firings of the co-precipitated hydroxides at 300, 350, and 400 C, including one in pure O2, failed to produce single phase cobaltate. Scanning electron microscopy showed all the sintered products to range over several orders of magnitude in agglomerate/particle size. Surface areas by BET were all in the range 40 to 110 m sq/g, equivalent to particles of 200 to 100 Angstrom diameter. The spinel diffraction line breadths were compatible with those approximate dimensions.

Singer, J.↗

Fluoride glass starting materials - Characterization and effects of thermal treatment

The production of heavy metal fluoride (HMF) glasses, and the effects of thermal treatments on the HMF glasses are investigated. ZrF4, BaF2, AlF3, LaF3, and NaF were utilized in the synthesis of zirconium-barium-lanthanum-aluminum-sodium fluoride glass. The purity of these starting materials, in particular ZrF4, is evaluated using XRD analysis. The data reveal that low temperature heating of ZrF4-H2O is effective in removing the water of hydration, but causes the production of ZrF4 and oxyfluorides; however, dehydration followed by sublimation results in the production of monoclinic ZrFe without water or oxyfluoride contaminants.

Chen, William↗

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗

Crystallization of BaF2-ZnF2-YbF3-ThF4 glass

The phases and the rates of crystallization in a Ba-Zn-Yb-Th fluoride glass were studied using differential scanning calorimetry, XRD, and observational and chemical SEM analyses. The crystallizing phases that were identified included a BaYbTh fluoride, ZnF2, and YbF3. The BaYbTh fluoride crystallized first at about 450 C, and ZnF2, which was excluded from this phase, crystallized at its surfaces. At higher temperatures, the BaYbTh fluoride phase decomposed partially to BaThF6 and YbF3 phases.

Garcia, Roberto↗

Crystallization and characterization of Y2O3-SiO2 glasses

Glasses in the yttria-silica system with 20-40 mol pct Y2O3 have been subjected to recrystallization studies after melting at 1900-2100 C in W crucibles in 1 and 50 atm N2. The TEM and XRD results obtained indicate the presence of the delta, gamma, gamma-prime, and beta-Y2Si2O7 crystalline phases, depending on melting and quenching conditions. Heat-treatment in air at 1100-1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristobalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.

Drummond, C. H., III↗

Improved synthesis of ceramic superconductors with alkaline earth peroxides - Synthesis and processing of Ba2YCu3O(7-x)

Synthesis processes for the preparation of ceramic conductors Ba2YCu3O(7-x) from BaO2 or BaCO3 in flowing O2 or N2 are described, and the characteristics of the materials produced in these processes are compared. Results of EDAX, XRD, SEM, and dc resistivity analyses demonstrated that superconducting materials made from BaO2 were more homogeneous, denser, and more metallic than materials produced from BaCO3, because of the higher reactivity of BaO2. Potential applications of this processes are discussed.

Hepp, A. F.↗

Gas atomization of cobalt ferrite-phosphate melts

XRD, Moessbauer spectroscopy, and EDXS have been used to characterize a rapidly-solidified (Co,Fe)3O4 spinel generated in a cobalt-iron-phosphate glass matrix by gas atomization of melts. Of the two compositions tested, that containing 20 mol pct P2O5 exhibited randomly-oriented ferrite crystallization whose growth appears to have been diffusion-controlled. Unlike the ferrite, in which the iron has both tetrahedral and octahedral coordination, the iron in the glassy matrix was primarily of distorted-octahedral coordination. Calculations indicate that the cooling rates obtained with oxide melts vary strongly with droplet size, but less strongly with melt temperature.

De Guire, Mark R.↗

Effect of the theta-alpha-Al2O3 transformation on the oxidation behavior of beta-NiAl+Zr

Isothermal oxidation of NiAl+Zr has been performed over the temperature range of 800-1200 C and studied by TGA, XRD, and SEM. A discontinuous decrease in growth rate of two orders of magnitude was observed at 1000 C due to the formation of alpha-Al2O3 from theta-Al2O3. This transformation also resulted in a dramatic change in the surface morphology of the scales, as a whisker topography was changed into a weblike network of oxide ridges and radial transformation cracks. It is believed that the ridges are evidence for a short-circuit outward aluminum diffusion growth mechanism that has been documented in a number of O-18 tracer studies.

Rybicki, George C.↗

Ceramic problems/challenges in high temperature oxide superconductors - Hysteretic force measurements as a new analysis tool

A technique is presented for analyzing high-temperature oxide superconductors using hysteretic magnetic force/distance measurements. Emphasis is placed on developing low weight, highly robust superconducting materials for space applications. Bi-Ca-Sr-Cu superconductors are prepared and characterized by standard techniques. It is found that standard techniques such as XRD, SEM, and TEM are insufficient to completely characterize superconductors. The magnetic properties of the superconductors are studied with the new technique, based on measuring the force between a magnet and the superconductor as a function of their separation.

Morgan, P. E. D.↗

Preparation of 110K (Bi, Pb)-Sr-Ca-Cu-O superconductor from glass precursor

The Bi1.5Pb0.5Sr2Ca2Cu3O(x) glass, prepared by rapid quenching of the melt, showed T(sub g) of 383 C, crystallization temperature of approx. 446 C, melting temperature of approx. 855 C, and bulk density of 5.69 g/cu. cm. in air. The as-quenched glass was oxygen deficient. On heating in O2, it showed a slow, irreversible, and continuous weight gain starting at approx. 530 C. The influence of annealing conditions on the formation of various phases was investigated by XRD and electrical resistivity measurements. The 110K-T(sub c) phase did not form below 840 C. The amount of this phase increased with the sintering time at 840 C. A sample annealed at 840 C for 243 h in air and furnace cooled showed the highest T(sub c)(R=0) of 107.2K and transition width delta T(sub c)(10 to 90 percent) of approx. 2 K.

Bansal, Narottam P.↗

Phillips CO-oxidation catalyts for long-lived CO2 lasers: Activity and initial characterization studies

Four different catalysts have been developed specifically for use in sealed carbon dioxide lasers. The catalysts have been designed to be low dusting, stable to shock and vibration, have high activity at low temperatures and have long active lifetimes. Measured global CO oxidation rates range from 1.4 to 2.2 cc CO converted per minute per gram of catalyst at ambient temperature. The catalysts also retain substantial activity at temperatures as low as -35 C. The Phillips laser catalysts are prepared in a variety of different shapes to meet the different pressure drop and gas flow profiles present in the many different styles of lasers. Each catalyst has been tested in sealed TEA lasers and has been shown to substantially increase the sealed life of the laser. Activity measurements made on the precious metal catalysts which were prepared with and without activity promoters showed that the promoter materials increase catalyst CO oxidation activity at least an order of magnitude at ambient temperature. Initial studies using H2 and CO chemisorption, X ray diffraction (XRD) and X ray photoelectron spectroscopy (XPS) have shown that the activity promoters do not significantly affect the precious metal crystallite size or the electronic structure around the precious metal. In addition, the formation or lack of formation of solid solutions between the precious metal and promoters has also been shown not to affect the activity of the promoted catalyst.

Kolts, J. H.↗

Stabilization of high T(sub c) phase in bismuth cuprate superconductor by lead doping

It has widely been ascertained that doping of lead in Bi:Sr:Ca:Cu:O systems promotes the growth of high T(sub c) (110 K) phase, improves critical current density, and lowers processing temperature. A systematic investigation is undertaken to determine optimum lead content and processing conditions to achieve these. A large number of samples with cationic compositions of Bi(2-x)Pb(x)Sr2Ca2Cu3 (x = 0.2 to 2.0) were prepared by conventional solid state reaction technique. Samples of all compositions were annealed together at a temperature and characterized through resistance-temperature (R-T) measurements and x ray diffraction (XRD) to determine the zero resistance temperature, T(sub c)(0) and to identify presence of phases, respectively. The annealing temperature was varied between 790 C to optimize processing parameters. Results are given. In brief, an optimum process is reported along with composition of leaded bismuth cuprate superconductor which yields nearly a high T(sub c) single phase with highly stable superconducting properties.

Gupta, Ram. P.↗

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗

Space manufacturing in an automated crystal growth facility

An account is given of a Space Station Freedom-based robotic laboratory system for crystal growth experiments; the robot must interface with both the experimental apparatus and such human input as may be required for control and display. The goal of the system is the simultaneous growth of several hundred protein crystals in microgravity. The robot possesses six degrees-of-freedom, allowing it to efficiently manipulate the cultured crystals as well as their respective growth cells; the crystals produced are expected to be of sufficiently high quality for complete structural determination on the basis of XRD.

Quinn, Alberta W.↗

Superconducting glass-ceramics in the Bi-Sr-Ca-Cu-O system

Differential thermal analysis, XRD, SEM, and resistivity measurements, have been used to study the recrystallization during various heat treatments of a Bi1.5SrCaCu2O(z) glass obtained by rapid quenching from the melt. Heating at 450 C formed the Bi(2+x)Sr(2-x)-CuO(z) solid solution designated 'R'. Between 765 and 845 C, R reacts slowly with the glass to form the 80 K superconductor Bi2(Sr,Ca)3Cu2O(z), together with CuO. Heating for 7 days at the higher temperature, followed by slow cooling, raised the temperature of zero resistance to 77 K.

De Guire, Mark R.↗

The effect of nitrogen on xenon ion engine erosion

Erosion studies were performed on a 30-cm diameter J-series ion engine modified for operation on xenon propellant. The erosion rates of molybdenum and tantalum badges placed at different locations within the discharge chamber were measured as a function of the percentage of nitrogen (by mass) added to the xenon propellant. Reductions in the erosion rates of these badges of a factor of 8 to 50 were observed at nitrogen addition fractions between 0.5 to 2.0 percent. Reductions in cathode-side baffle erosion were achieved by adding nitrogen to the xenon propellant or by increasing the cathode orifice diameter. Analyses show that no significant degradation in ion engine performance should be expected at these nitrogen mass fractions. XRD, XPS and Auger analyses indicate the existence of nitrogen and nitrides in the surface of some but not all of the badges used in the tests where nitrogen was added to the xenon. Difficulty in identifying surface nitrides in the samples may be due to the existence of surface oxides and contaminants, or to the small thicknesses of the nitride layers.

Garner, Charles E.↗