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Bulk specimens (0.4-4 g mass) of the alloy Pd40Ni40P20 have been undercooled consistently to the glass state, with no detectable superficial crystallinity, in a molten flux of dehydrated boron oxide. The minimum dimension of the most massive glass specimen, so formed, was 1.0 cm. The absence of crystallinity in the specimens was confirmed by X-ray diffraction, scanning electron microscopy, and calorimetry.
The potential for silicate-carbon dioxide reactions as a geochemical weathering agent on Venus was studied. A tholetitic basalt close to the composition determined by the XRF experiment at the Venera 14 sites was subjected to high temperature and pressure (with pure CO2 as the pressure medium) for varying time durations. The starting basalt material and the run products were examined optically and by X-ray diffraction and electron microscopy. The kinetics of the silicate-carbonate reactions is discussed. A study to elucidate details of impact processes and to assess the effects of impact cratering on planetary evolution is mentioned.
Polycrystalline Co-49.3 at. pct Al, which had been extruded at 1505 K, was examined using transmission electron microscopy. Diffraction contrast analysis showed that b = 100 as well as b = 111 line dislocations contribute to elevated temperature deformation in CoAl. Therefore, it was concluded that sufficient slip systems exist in CoAl to allow for general plasticity in the absence of diffusional mechanisms. Line dislocations of the type b = 001 were observed on both 110 and 100 planes while b = 111 line dislocations were observed on 1 -1 0 planes.
Four phases are observed in superconducting Bi-Ca-Sr-Cu-O samples. The superconducting phase, with onset temperature near 120 K, is a 15.4-A-layered compound with composition near Bi2Ca1Sr2Cu2O9 and an A-centered orthorhombic unit subcell 5.41 x 5.44 x 30.78 A. X-ray diffraction and electron microscopy data are consistent with a structure of alternating perovskite and Bi2O2 layers. High-resolution transmission electron microscopy images reveal a b-axis superstructure of 27.2 A, numerous (001) stacking faults, and other defects.
Epitaxial CdTe has been grown on both (100)GaAs/Si and (111)GaAs/Si substrates. A combination of molecular beam epitaxy (MBE) and metalorganic chemical vapor deposition (MOCVD) has been employed for the first time to achieve this growth: the GaAs layers are grown on Si substrates by MBE and the CdTe film is subsequently deposited on GaAs/Si by MOCVD. The grown layers have been characterized by X-ray diffraction, scanning electron microscopy, and photoluminescence.
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.
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.
Pseudotachylite is known to occur in a variety of geologic settings including thrust belts (e.g., the Alps and the Himalayas) and impact craters such as Roter Kamm, Namibia. Controversy exists, however, as to whether pseudotachylite can be produced by shock brecciation as well as by tectonic frictional melting. Also open to debate is the question of whether pseudotachylites form by frictional fusion or by cataclasis. It was speculated that the pseudotachylite at Roter Kamm was formed by extensional settling and adjustment of basement blocks during 'late modification stage' of impact. The occurrence of pseudotachylite in association with rocks resembling quenched glass bombs and melt breccias in a relatively young crater of known impact origin offers a rare opportunity to compare features of these materials. Petrographic, x-ray diffraction, and electron microprobe analyses of the impactites and pseudotachylites are being employed to determine the modes of deformation and to assess the role of frictional melting and comminution of adjacent target rocks.
The objective of this investigation is to develop a technique with which refractory metal carbide samples can be exposed to hydrogen containing gases at high temperatures, and to use various microstructural and analytical techniques to determine the chemical and rate processes involved in hydrogen degradation in these materials. Five types of carbides were examined including WC, NbC, HfC, ZrC, and TaC. The ceramics were purchased and were all monolithic in nature. The temperature range investigated was from 850 to 1600 C with a hydrogen pressure of one atmosphere. Control experiments, in vacuum, were also conducted for comparison so that the net effects due to hydrogen could be isolated. The samples were analyzed prior to and after exposure. Gas samples were collected in selected experiments and analyzed using gas chromography. Characterization of the resulting microstructure after exposure to hydrogen was conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. The ceramics were purchased and were all monolithic in nature. It was found that all samples lost weight after exposure, both in hydrogen and vacuum. Results from the microstructure analyses show that the degradation processes are different among the five types of ceramics involved. In addition, the apparent activation energy for the degradation process is a function of temperature even within the same material. This indicates that there are more than one mechanism involved in each material, and that the mechanisms are temperature dependent.
Polycrystalline samples of the chalcopyrites CuInS2, CuInSe2, and CuInSSe were prepared from stoichiometric mixtures of the pure elements by microwave irradiation. The reactions were performed in sealed quartz tubes in as few as 3 minutes. The products were analyzed by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, and X-ray photoelectron spectroscopy. The surface morphology and shape of the particles produced by this method suggest that the products are formed from liquid melts. This method could be applied to the production of bulk chalcopyrite as sources for thin film growth.
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This abstract reports results of an experimental study of the chemical weathering of pyrite (FeS2) under Venus-like conditions. This work, which extends the earlier study by Fegley and Treiman, is part of a long range research program to experimentally measure the rates of thermochemical gas-solid reactions important in the atmospheric-lithospheric sulfur cycle on Venus. The objectives of this research are (1) to measure the kinetics of thermochemical gas-solid reactions responsible for both the production (e.g., anhydrite formation) and destruction (e.g., pyrrhotite oxidation) of sulfur-bearing minerals on the surface of Venus and (2) to incorporate these and other constraints into holistic models of the chemical interactions between the atmosphere and surface of Venus. Experiments were done with single crystal cubes of natural pyrite (Navajun, Logrono, Spain) that were cut and polished into slices of known weight and surface area. The slices were isothermally heated at atmospheric pressure in 99.99 percent CO2 (Coleman Instrument Grade) at either 412 C (685 K) or 465 C (738 K) for time periods up to 10 days. These two isotherms correspond to temperatures at about 6 km and 0 km altitude, respectively, on Venus. The reaction rate was determined by measuring the weight loss of the reacted slices after removal from the furnace. The reaction products were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy on the SEM.
The objectives of this investigation are to expose heat resistant alloys to hydrogen at elevated temperatures and to use various microstructural and analytical techniques to determine the chemical and rate process involved in degradation of these materials due to hydrogen environment. Inconel 718 and NASA-23 (wrought and cast) are candidate materials. The degradation of these materials in the presence of 1 to 5 atmospheric pressure of hydrogen from 450 C to 1100 C was examined. The hydrogen facility at Auburn University was used for this purpose. Control experiments were also conducted wherein the samples were exposed to vacuum so that a direct comparison of the results would separate the thermal contribution from the hydrogen effects. The samples were analyzed prior to and after exposure. A residual gas collection system was used to determine the gaseous species produced by any chemical reaction that may have occurred during the exposure. Analysis of this gas sample shows only the presence of H2 as expected. Analyses of the samples were conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. There appears to be no change in weight of the samples as a result of hydrogen exposure. In addition no visible change on the surface structure was detected. This indicates that the materials of interest do not have strong interaction with hot hydrogen. This is consistent with the microstructure results.
The burn rates of the pyrotechnic TiH2/KClO4/Viton with a mass ratio of 30/65/5 have been measured as a function of pressure in nitrogen up to 312 MPa(45 Kpsi). The burn rates were fit to R = a pn, with a = 2.055 cm/sec/MPan and n = 0.472 between 0.15 MPa (22 psi) and 21.6 MPa (3.13 Kpsi) and a = 4.38 cm/sec/MPan and n = 0.266 between 70 MPa (10.15 Kpsi) and 312 MPa (45.25 Kpsi). The decrease in slope at the higher pressures is attributed to a diffusion limited reaction. No acoustically driven flame instabilities or large conductive-to-convective burn transitions were observed. Solid reaction products were analyzed by x-ray diffraction and scanning electron microscopy (SEM). X-ray diffraction detected only TiO2 and KC1. SEM showed that the particle size of the reaction products increased as the nitrogen pressure increased. There were no anomalous characteristics of the burn of this pyrotechnic that could be interpreted as a cause of the o-ring blow-by problem in the forward shear bolt assembly. Three NASA SKD26100098-301 pressure cartridges were fired into a fixed volume vessel that was sealed with an O-ring. A maximum pressure of 181.7 MPa(26,350 psi) was reached in around 100 ,mu sec for two shots fired into a volume of 16.3 cm3(0.996 in3). A maximum pressure of 33,460 psi was reached for one shot fired into a volume of 9.55 cm3(0.583 in3). The O-ring burned through on one shot in the larger volume and leaked on the other two thereby simulating the effects of an O-ring leak. The results imply that the piston in the shear bolt assembly would receive a large impulse even if there was a leak in an O-ring seal.
Long lengths of (Bi,Pb)2Sr2Ca2Cu3O(x) tapes made by powder-in-tube processing have been wound into coils. Performance of the coils has been measured at temperatures of 4.2 to 77 K, and microstructures have been examined by x-ray diffraction and electron microscopy and then related to superconducting properties. A summary of recent results and an overview of future goals are presented.
The high strength, low density, and good corrosion resistance of Ti-based alloys make them candidate materials for a number of applications in the aerospace industry. A major limitation in the use of these alloys in the advanced hypersonic flight vehicle program is their susceptibility to hydrogen embrittlement. This study focuses on the hydrogen sensitivity of TIMETAL 21S beta-Ti alloy. The material received was in the form of grip-ends of failed tensile test samples which had been exposed to different charging conditions (combinations of hydrogen pressure and temperature). The samples received, the charging conditions, and their fracture mode are discussed. It can be seen that the fracture behavior changes from ductile to brittle with increasing hydrogen content, but the transition in behavior occurs for a small increase in hydrogen concentration. The aim of this program was to assess the microstructural differences between the ductile and brittle alloys to ascertain the embrittlement mechanism. A range of tools which included x-ray diffraction, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used.
Phthalocyanine is a very stable organic material in the atmosphere and has been used in numerous applications, such as optical switching and optical storage devices. Although this material has already been discovered for several decades and has had extensive studies conducted on it, many properties still need to be better understood, for example, the mechanisms of forming different solid phases and of changing film morphology by external forces. Phthalocyanine has two preferred solid phases (alpha and beta phases) for which the crystal structures, surface morphology and optical properties are different. In order to investigate these phenomena and the relationship among them, phthalocyanine films have been synthesized by vapor deposition on quartz substrates with and without an external electrical field. Some substrates were coated with a very thin gold film for the electrical field. These films have been characterized using x-ray diffraction, scanning electron microscopy, Fourier transfer infrared spectroscopy, and Z-scan technique. The films have excellent chemical and thermal stability. However, the surface of these films grown without the electrical field shows flower-like morphology. When films are deposited under an electrical field (approximately 3000 V/cm), an aligned structure is revealed on the surface. A comparison of the structure, morphology, optical properties, and the growth mechanism for these films with and without an electrical field will be discussed.
Solid oxide fuel cells (SOFCs) have been considered as premium future power generation devices because they have demonstrated high energy-conversion efficiency, high power density, and extremely low pollution, and have the flexibility of using hydrocarbon fuel. The Solid-State Energy Conversion Alliance (SECA) initiative, supported by the U.S. Department of Energy and private industries, is leading the development and commercialization of SOFCs for low-cost stationary and automotive markets. The targeted power density for the initiative is rather low, so that the SECA SOFC can be operated at a relatively low temperature (approx. 700 C) and inexpensive metallic interconnects can be utilized in the SOFC stack. As only NASA can, the agency is investigating SOFCs for aerospace applications. Considerable high power density is required for the applications. As a result, the NASA SOFC will be operated at a high temperature (approx. 900 C) and ceramic interconnects will be employed. Lanthanum chromite-based materials have emerged as a leading candidate for the ceramic interconnects. The interconnects are expected to co-sinter with zirconia electrolyte to mitigate the interface electric resistance and to simplify the processing procedure. Lanthanum chromites made by the traditional method are sintered at 1500 C or above. They react with zirconia electrolytes (which typically sinter between 1300 and 1400 C) at the sintering temperature of lanthanum chromites. It has been envisioned that lanthanum chromites with lower sintering temperatures can be co-fired with zirconia electrolyte. Nonstoichiometric lanthanum chromites can be sintered at lower temperatures, but they are unstable and react with zirconia electrolyte during co-sintering. NASA Glenn Research Center s Ceramics Branch investigated a glycine nitrate process to generate fine powder of the lanthanum-chromite-based materials. By simultaneously doping calcium on the lanthanum site, and cobalt and aluminum on the chromium site, we could sinter the materials below 1400 C. The doping concentrations were adjusted so that the thermal expansion coefficient matched that of the zirconia electrolyte. Also, the investigation was focused on stoichiometric compositions so that the materials would have better stability. Co-sintering and chemical compatibility with zirconia electrolyte were examined by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy (line scanning and dot map). The results showed that the materials bond well, but do not react, with zirconia electrolyte. The electric conductivity of the materials measured at 900 C in air was about 20 S/cm.