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At least 127 records · Page 7

Effect of processing parameters on the characteristics of high-Tc superconductor YBa2Cu3Oy

SEM, thermogravimetric analysis, powder X-ray diffraction,and measurements of electrical resistivity and magnetic susceptibility, are presently used to characterize the influence of sintering temperature, sintering and annealing atmospheres, and quench-rate on the properties of the YBa2Cu3Oy superconducting oxide. It is established that annealing in oxygen, together with slow cooling rates, are required for preparation of high-Tc superconductors with sharp transitions; rapid quenching from high temperature does not yield good superconductors, due to low oxygen content.

Bansal, Narottam P.↗

Reactions of silicon-based ceramics in mixed oxidation chlorination environments

The reaction of silicon-based ceramics with 2 percent Cl2/Ar and 1 percent Cl2/1 percent to 20 percent O2/Ar at 950 C was studied with thermogravimetric analysis and high-pressure mass spectrometry. Pure Si, SiO2, several types of SiC, and Si3N4 were examined. The primary corrosion products were SiCl4(g) and SiO2(s) with smaller amounts of volatile silicon oxychlorides. The reactions appear to occur by chlorine penetration of the SiO2 layer, and gas-phase diffusion of the silicon chlorides away from the sample appears to be rate limiting. Pure SiO2 shows very little reaction with Cl2, SiC with excess Si is more reactive than the other materials with Cl2, whereas SiC with excess carbon is more reactive than the other materials with Cl2/O2. Si3N4 shows very little reaction with Cl2. These differences are explained on the basis of thermodynamic and microstructural factors.

Marra, John E.↗

The behavior of SiC and Si3N4 ceramics in mixed oxidation/chlorination environments

The behavior of silicon-based ceramics in mixed oxidation/chlorination environments was studied. High pressure mass spectrometry was used to quantitatively identify the reaction products. The quantitative identification of the corrosion products was coupled with thermogravimetric analysis and thermodynamic equilibrium calculations run under similar conditions in order to deduce the mechanism of corrosion. Variations in the behavior of the different silicon-based materials are discussed. Direct evidence of the existence of silicon oxychloride compounds is presented.

Marra, John E.↗

The 3F condensation polyimides: Review and update

Nine new condensation polyimides containing the phenyltrifluoroethylidene (3F) linkage were synthesized by the amic-acid route. Several other polyimides, including some with hexafluoroisopropylidene (6F) linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sub g), thermogravimetric analysis (TGA), and isothermal weight loss data (at 316, 371, and 371 C under 0.5 MPa air pressure) were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin disks. The disks were also characterized by T sub g's and 316 and 371 C isothermal weight losses. The film study identified two new polyimides with T sub g's greater than 371 C and two new polyimides with low rates of weight loss. The resin disks exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to molecular degradation induced during preparation of the molding powders. The overall results indicate that polyimides containing the 3F linkage have T sub g's and thermo-oxidative stability comparable to polyimides containing the 6F group. Alternate technology was also shown by the synthesis of two new polyalkyl substituted 3F diamines and five more new 3F polymers. Their potential as photoresists was demonstrated by T sub g advancement after ultraviolet exposure. Last, four U.S. patents on 3F monomers and polymers were issued and up to eight more are pending.

Alston, William B.↗

Novel polyimide compositions based on 4,4': Isophthaloyldiphthalic anaydride (IDPA)

A series of twelve high temperature, high performance polyimide compositions based on 4,4'-isophthaloyl diphthalic anhydride (IDPA) was prepared and characterized. Tough, film-forming, organic solvent-insoluble polyimides were obtained. Three materials were semicrystalline. Several gave excellent long-term thermooxidative stability by isothermal thermogravimetric analysis (ITGA) at 300 C and 350 C in air when compared to Kapton H film (duPont). One extensively studied material displayed different levels of semicrystallinity over a wide range of final cure time/temperatures. The polyimide from IDPA and 1,3-bis (4-aminophenoxy 4'-benzoyl) benzene exhibited multiple crystallization and melting behavior, implying the existence of two kinetic and two thermodynamic crystallization and melting transitions by differential scanning calorimetry (DSC).

Pratt, J. Richard↗

Electrocatalysis for oxygen electrodes in fuel cells and water electrolyzers for space applications

The lead ruthenate pyrochlore Pb2Ru2O6.5, in both high- and low-area forms, has been characterized using thermogravimetric analysis, X-ray photoelectron spectroscopy, X-ray diffraction, cyclic voltammetry, and O2 reduction and generation kinetic-mechanistic studies. Mechanisms are proposed. Compounds in which part of the Ru is substituted with Ir have also been prepared. They exhibit somewhat better performance for O2 reduction in porous, gas-fed electrodes than the unsubstituted compound. The anodic corrosion resistance of pyrochlore-based porous electrodes was improved by using two different anionically conducting polymer overlayers, which slow down the diffusion of ruthenate and plumbate out of the electrode. The O2 generation performance was improved with both types of electrodes. With a hydrogel overlayer, the O2 reduction performance was also improved.

Prakash, Jai↗

Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo intermetallic alloy

Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using x ray diffraction techniques, electron microprobe analysis, and energy dispersive x ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

Wallace, Terryl A.↗

Effect of molecular weight on polyphenylquinoxaline properties

A series of polyphenyl quinoxalines with different molecular weight and end-groups were prepared by varying monomer stoichiometry. Thus, 4,4'-oxydibenzil and 3,3'-diaminobenzidine were reacted in a 50/50 mixture of m-cresol and xylenes. Reaction concentration, temperature, and stir rate were studied and found to have an effect on polymer properties. Number and weight average molecular weights were determined and correlated well with viscosity data. Glass transition temperatures were determined and found to vary with molecular weight and end-groups. Mechanical properties of films from polymers with different molecular weights were essentially identical at room temperature but showed significant differences at 232 C. Diamine terminated polymers were found to be much less thermooxidatively stable than benzil terminated polymers when aged at 316 C even though dynamic thermogravimetric analysis revealed only slight differences. Lower molecular weight polymers exhibited better processability than higher molecular weight polymers.

Jensen, Brian J.↗

The formation and study of titanium, zirconium, and hafnium complexes

Research involves the preparation and characterization of a series of Ti, Zr, Hf, TiO, and HfO complexes using the poly(pyrazole) borates as ligands. The study will provide increased understanding of the decomposition of these coordination compounds which may lead to the production of molecular oxygen on the Moon from lunar materials such as ilmenite and rutile. The model compounds are investigated under reducing conditions of molecular hydrogen by use of a high temperature/pressure stainless steel autoclave reactor and by thermogravimetric analysis.

Wilson, Bobby↗

Synthesis and properties of Ti-substituted goethites and hematites

The objective was to synthesize Ti-substituted goethites and hematites and to characterize them using x-ray diffraction, thermogravimetric analysis, coulimetry, optical and Mossbauer spectroscopies, and magnetic data in order to determine the evidence of Ti substitution for Martian spectral data. Evidence is provided that up to 4 mole percent can be incorporated into the goethite structure during the low temperature synthesis. Because the spectral data in the visible and near-IR are not sensitive to the degree of Ti-substitution in goethites and hematites, such data cannot be used to infer the presence or absence of Ti substitution in Martian hematites and goethites.

Vempati, R. K.↗

Chemical compatibility of cartridge materials

This twelve month progress report deals with the chemical compatibility of semiconductor crystals grown in zero gravity. Specifically, it studies the chemical compatibility between TZM, a molybdenum alloy containing titanium and zirconium, and WC 103, a titanium alloy containing Niobium and Hafnium, and Gallium arsenide (GaAs) and Cadmium Zinc Tellurite (CdZnTe). Due to the health hazards involved, three approaches were used to study the chemical compatibility between the semiconductor and cartridge materials: reaction retort, thermogravimetric analysis, and bulk cylindrical cartridge containers. A scanning electron microscope with an energy dispersive X-ray analyzer was used to examine all samples after testing. The first conclusion drawn is that reaction rates with TZM were not nearly as great as they were with WC 103. Second, the total reaction between GaAs and WC 103 was almost twice that with TZM. Therefore, even though WC 103 is easier to fabricate, at least half of the cartridge thickness will be degraded if contact is made with one of the semiconductor materials leading to a loss of strength properties.

Wilcox, Roy C.↗

Oxidation characteristics of Beta-21S in air in the temperature range 600 to 800 C

The metastable beta-Ti alloy Beta-21S, Ti-15Mo-2.7Nb-3Al-0.2Si (weight percent), has been proposed as a candidate for use in metal matrix composites in future hypersonic vehicles. The present study investigated the oxidation behavior of Beta-21S over the temperature range 600 C to 800 C. Oxidation weight gain was evaluated using thermogravimetric analysis. Oxidized specimens were evaluated using x ray diffraction techniques, scanning electron microscopy, energy dispersive x ray analysis, and electron microprobe analysis to identify oxidation products and evaluate oxidation damage to the alloy.

Wallace, Terryl A.↗

Oxidation-chlorination of binary Ni-Cr alloys in flowing Ar-O2-Cl2 gas mixtures at 1200 K

Nickel-chromium alloys are resistant to oxidation because of the selective oxidation of chromium to form a protective Cr2O3 scale. In chlorine-containing environments, volatile corrosion products can also be formed. The mixed oxidation-chlorination of Ni-4.5Cr, Ni-13.8Cr, and Ni-26.5Cr (by weight) alloys in Ar-O2-Cl2 gas mixtures is investigated using thermogravimetric analysis and atmospheric-pressure-sampling mass spectrometry, followed by examination of the corrosion products using scanning electron microscopy and X-ray diffraction analysis. The overall kinetics of the corrosion are affected by the relative amounts of oxides and chlorides formed and the composition of the oxide corrosion products.

Mcnallan, M. J.↗

Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo

Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using X-ray diffraction techniques, electron microprobe analysis, and energy dispersive X-ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

Wallace, T. A.↗

Polyimides Made From 4,4'-Isophthaloyldiphthalic Anhydride

High-performance, thermoplastic, amorphous, and semicrystalline materials obtained. In experiments, twelve high-temperature, high-performance polyimide compositions based on 4,4'-isophthaloyldiphthalic anhydride (IDPA) prepared and characterized. Tough, film-forming, polyimides insoluble in organic solvents obtained in most cases. Three materials semicrystalline. Materials offer potential for development of semicrystalline polyimides having enhanced resistances to solvents and caustic chemicals, higher tensile strengths and moduli, enhanced thermo-oxidative stabilities below their melting temperatures, and enhanced melt processability, especially when heated to melting temperatures. Several exhibited excellent long-term thermo-oxidative stability when subjected to isothermal thermogravimetric analysis (ITGA) at temperatures of 300 degrees C and 350 degrees C in air. One area of application, manufacturing of lighter and stronger aircraft and spacecraft structures.

Pratt, J. Richard↗

Material selection and evaluation of new encapsulation compounds for electric cables for launch support system

Eight urethane compounds were evaluated as possible replacement for the existing encapsulating compoounds for electrical cables for the Launch Support System at Kennedy Space Center (KSC). The existing encapsulating compound, PR-1535, contains the curative MOCA 4-4'-Methylene-BIS (2-chloroaniline), which is a suspect carcinogen and hence may be the subject of further restrictions of its use by the Occupational Safety and Health Administration (OSHA). The samples made in the configuration of cable joints and in the form of disks were evaluated for flammability and hypergolic compatibility. These also underwent accelerated weatherability tests that measured the residual hardness of the exposed samples. Three candidates and the existing compound passed the hardness test. Of these, only one candidate and the existing compound passed the flammability test. The thermal and hydrolytic stability (weatherability) of these samples was studied using thermogravimetric analysis (DSC) techniques. The TMA and DSC data correlated with the residual hardness data; whereas, the TGA data showed no correlation. A hypergolic compatibility test will be conducted on the compound V-356-HE80, which passed both the flammability and accelerated weatherability tests.

Ray, Asit K.↗

Oxidation characteristics of Ti-33Al-6Nb-1.4Ta

Static oxidation kinetics of the gamma titanium-aluminide alloy Ti-33Al-6Nb-1.4Ta (wt pct) have been investigated in air from 700 to 1000 C and in oxygen from 800 to 1000 C using thermogravimetric analysis. The oxidation kinetics were controlled by the presence of alumina for all oxygen exposures and in air below 800 C, while the kinetics in air above 800 C were more complex. Oxidation products were identified using X-ray diffraction techniques. Oxide scale morphology was examined by SEM and TEM of the surfaces and across sections of oxidized specimens. The oxidation products formed depended on the exposure: Al2O3 and TiO2 were identified on all specimens exposed in and air and oxygen; the nitride phases TiN and Ti2AlN were also found on specimens exposed in air.

Wallace, T. A.↗

Polyimides containing pendent trifluoromethyl groups

Several new polyimides containing trifluoromethyl groups were prepared from the reaction of various aromatic dianhydrides and two new diamines containing trifluoromethyl groups, 4,4'-bis(3-amino-5-trifluoromethylphenoxy)biphenyl and l,4-bis(3-amino-5-trifluoromethylphenoxy)benzene. The diamines were prepared from the aromatic nucleophilic displacement of the disodium salts of 4,4'-biphenol or hydroquinone with 3,5-dinitrobenzotrifluoride followed by hydrogenation of the resultant dinitro compounds. The thermally cured polyimides exhibited glass transition temperatures between 186 and 262 C. By thermogravimetric analysis, the polyimides exhibited 5 percent weight losses at 484-527 C in nitrogen and 452-506 C in air.

Havens, S. J.↗