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At least 1,171 records · Page 65

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NASA NTRS1987

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↗

NASA NTRS1988

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.↗

NASA NTRS1988

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↗

NASA NTRS1988

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↗

NASA NTRS1988

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.↗

NASA NTRS1989

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.↗

NASA NTRS1989

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.↗

NASA NTRS1989

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.↗

NASA NTRS1989

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.↗

NASA NTRS1990

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.↗

NASA NTRS1990

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.↗

NASA NTRS1989

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Bansal, Narottam P.↗

NASA NTRS1989

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.↗

NASA NTRS1990

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.↗

NASA NTRS1990

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.↗

NASA NTRS1990

Characterization of LaRC-TPI 1500 powders - A new version with controlled molecular weight

The crystallization behavior and the melt flow properties of two batches of 1500 series LaRC-TPI polymers have been investigated. The characterization methods include DSC, XRD, and melt rheology. The as-received materials posses initial crystalline melting peak temperatures of 295 and 305 C, respectively. These materials are less readily recrystallizable at elevated temperatures when compared to other semicrystalline thermoplastics. For the samples annealed at temperatures below 330 C, a semicrystalline polymer can be obtained. On the other hand, a purely amorphous structure is realized in samples annealed at temperatures above 330 C. The viscoelastic properties at elevated temperatures below and above T(g)s of the polymers were measured. Information with regard to the molecule sizes and distributions in these polymers were also extracted from melt rheology.

Hou, T. H.↗

NASA NTRS1991

Crystallization and characterization of Y2O3-SiO2 glasses

Glasses in the yttria-silica system with 20 to 40 mol pct Y2O3 were subjected to recrystallization studies after melting at 1900 to 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 to 1600 C increased the amount of crystallization, and led to the formation of Y2SiO5, cristabalite, and polymorphs of Y2Si2O7. Also investigated were the effects of 5 and 10 wt pct zirconia additions.

Drummond, Charles H., III↗

NASA NTRS1990

Static compression of iron to 300 GPa and Fe(0.8)Ni(0.2) alloy to 260 GPa - Implications for composition of the core

Results are reported on a room temperature static compression study of iron and the Fe(0.8)Ni(0.2) alloy to above 260 GPa, which provide direct pressure-volume measurements on geophysically important materials at the conditions close to those at the inner core boundary. The diffraction patterns obtained by XRD indicate that pure iron remains in the hcp structure to 304 GPa and that Fe(0.8)Ni(0.2) is stable to at least 255 GPa. The results of this study, in conjunction with work at higher temperatures, will make it possible to address directly the question of the composition of the inner core with a level of certainty that were previously applicable only to the mantle.

Mao, H. K.↗