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At least 307 records · Page 17

Materials science and manufacturing in space: The NBS program of ground based research

National Bereau of Standards work for NASA in support of NASA's Space Processing Program is described. The objectives of the NBS program are to perform ground-based studies of those aspects of space that could possibly provide a unique environment for making materials more perfect or more pure. The approach taken deals primarily with experimental and theoretical studies of the possible effects of the absence of gravitational forces on those materials preparation processes where the presence of gravity may be important in reducing perfection or purity. The materials preparation processes studied comprise 6 tasks in the areas of crystal growth, purification and chemical processing, and the preparation of composites. They are: (1) crystal perfection in Czochralski growth; (2) evaporative preparation of ultrahigh purity materials; (3) vacuum effects in the preparation of composite materials; (4) melt shape in weightless crystal growth; (5) vapor transport synthesis and crystal growth of oxides; and (6) surface traction and other surface phenomena.

Passaglia, E.↗

Study of the thermal degradation mechanism of a composite propellant

The current experimental program was designed to systematically investigate the role of the oxidizer in the thermal degradation process of composite propellants. The scanning electron microscope (SEM) was used to examine the failure sites in thermally degraded propellant samples. The formulation variables tested were oxidizer purity, oxidizer particle size, and oxidizer to binder bonding agent. The binder, a saturated hydrocarbon, was kept constant throughout the experiments. The oxidizers were: AP, chlorate-doped AP, arsenate-doped AP, and phosphate-doped AP. The oxidizer particle size distribution was 60% of the large fraction and 40% of the small fraction. The bonding agent, when present, was used at the 0.15% level. The data showed that both the oxidizer purity and particle size had an important affect on the thermal degradation process. The affect of the oxidizer particle size was more noticeable at the higher temperature and stress levels. An examination of the failure site, by SEM, of propellants subject to these latter conditions indicated that the fracturing of the large oxidizer particles led to the propellant cracking.

Schmidt, W. G.↗

Fused silica reflecting heat shields for outer planet entry probes

The development of slip-cast fused silica is discussed as a heat shield designed to meet the needs of outer-planet entry probes. The distinguishing feature of silica is its ability to reflect the radiation imposed by planetary-entry environments. This reflectivity is particularly sensitive to degradation by the presence of trace amounts of contaminants introduced by the starting materials or by processing. The microstructure of a silica configuration also significantly influences the reflectivity and other thermomechanical properties. The processing techniques attendant on controlling microstructure while maintaining purity are discussed. The selection of a starting material of essential purity precludes the use of purified natural quartz and requires the use of synthetic fused silica. The silica is characterized in a limited combined heating test environment. The surface mass loss is controlled by liquid runoff from a relatively low-temperature melt layer; the reflectance is basically maintained and the material achieves a surprisingly high heat of ablation.

Congdon, W. M.↗

Effect of processing variables on the thermophysical properties of polybenzimidazole foams

The relationships are described among prepolymer purity, processing parameters, and additives to the thermophysical and chemical properties of polybenzimidazole foams in the density range from 24 to 80 kg/cu m. Foam properties are shown to be affected by differences in prepolymer purity, curing schedule, and the presence of additives in the foam. High-temperature compressive properties were improved by postcuring at 527 C. Surfactant additives were found to improve uniformity of cell size. Foams were characterized according to high-temperature mechanical properties, density, porosity, thermal diffusivity, thermal conductivity, and specific heat.

Kourtides, D. A.↗

Low cost processes for solar-grade silicon

Upgrading metallurgical grade silicon is being pursued in four associated areas in order to improve the purity of the normally 98% material. The first two work areas involve purification of raw materials entering the process in addition to upgrading the arc furnace itself. The second two areas of process upgrading comprise improving the purity of the silicon after it leaves the arc furnace by reactive gas blowing and unidirectional freezing. The best cell produced to date was fabricated from MG-Si that had been blown with an O2-Cl2 mixture, unidirectionally solidified, and 6-float-zone passed (to determine a base boron level of 0.04 ohm/cm). The cell showed a 10.7% AMO efficiency. In the other processes category, the use of silicates as a silicon source and of electrolysis as a process were studied. The best electrolytic process uses a 1000 C fused salt of silica in cryolite.

Hunt, L. P.↗

Space processing of chalcogenide glass

The manner in which the weightless, containerless nature of in-space processing can be successfully utilized to improve the quality of infrared transmitting chalcogenide glasses was investigated. The following conclusions were reached: (1) Laboratory experiments have established the techniques, processes and equipment necessary for the production of high purity chalcogenide glasses. (2) Processing techniques have been successfully adopted for Ge28Sb12Se60 glass in a 1-g environment. (3) The Ge28Sb12Se60 glasses that have been processed have optical transmission around 63% (5 mm thick). (4) Laboratory experiments have established that the use of precursor materials in powdered form increases the oxygen contamination of the processed glass. This indicates that high purity precursor materials in bar or pellet form should be used. (5) Modifications were made on the MSFC acoustic levitator in an attempt to improve levitation stability during long-time experiments. Room temperature experiments on As2S3 glasses and high temperature experiments on polystyrene were conducted.

Ali, M. A.↗

Fractography of the high temperature hydrogen attack of a medium carbon steel

Results are reported for an experimental study of the microscopic fracture processes associated with hydrogen attack of a commercially produced plain carbon steel in a well-controlled high-temperature hydrogen environment of high purity. In the experiments, sheet samples were exposed to laboratory-grade hydrogen at a pressure of 3.5 MN/sq m and a temperature of 575 C. The fractography of gas-filled fissures and failed tension specimens is analyzed in an effort to identify any predominant microstructural defect associated with fissure formation, the prevalent modes of fracture, and the contribution of gas-filled fissures to the overall failure process. It is found that the tensile properties of the examined steel were significantly degraded after as few as 136 hr of exposure to a high-purity hydrogen atmosphere at 575 C; that the yield strength, ultimate strength, and elongation at fracture were all reduced progressively with increasing exposure time; and that the yield and ultimate strengths were reduced more than 40% after 408 hr while elongation was reduced to less than 2%.

Nelson, H. G.↗

The preparation of calcium superoxide at subambient temperatures and pressures

The effects of disproportionations at lower temperatures and also of a range of reaction chamber pressures on the preparation of calcium superoxide, Ca(O2)2, from calcium peroxide diperoxyhydrate were studied. About 60% purity of product was obtained by a disproportionation procedure. The significance of features of this procedure for a prospective scale-up of the mass prepared in a single experiment is considered. The optimum pressure for product purity was determined, and the use of a molecular sieve desiccant is described.

Ballou, E. V.↗

Development of doped-germanium photoconductors for astronomical observations at wavelengths from 30 to 120 micrometers

Technology was developed for production of doped-germanium detectors which have optimized performance in the 30- to 120-micrometer wavelength range and are capable of achieving the objectives of the Infrared Astronomy Satellite space mission. The work of this phase was divided into the following major tasks: (1) growth of Ge:Ga crystals from high-purity starting material with Ga concentrations different from that previously produced, and development of a zone leveling method to produce a uniform Ga doping concentration; (2) growth of uncompensated Ge:Be crystals from high-purity starting material with a range of Be concentrations between 10 to the 14th power and 10 to the 16th power atoms/cubic cm; (3) evaluation of crystals by means of Hall effect and resistance measurements as a function of temperature; (4) fabrication and test of detectors made from both Ge:Be and Ge:Ga crystals to determine the relative performance between different crystals. Correlation of detector test data with material evaluation data and analysis of how to further optimize detector performance.

Bratt, P. R.↗

Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions

X-ray photoelectron spectroscopy was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

Wheeler, D. R.↗

Passive particle dosimetry

Present methods of dosimetry are reviewed with emphasis on the processes using silver chloride crystals for ionizing particle dosimetry. Differences between the ability of various crystals to record ionizing particle paths are directly related to impurities in the range of a few ppm (parts per million). To understand the roles of these impurities in the process, a method for consistent production of high purity silver chloride, and silver bromide was developed which yields silver halides with detectable impurity content less than 1 ppm. This high purity silver chloride was used in growing crystals with controlled doping. Crystals were grown by both the Czochalski method and the Bridgman method, and the Bridgman grown crystals were used for the experiments discussed. The distribution coefficients of ten divalent cations were determined for the Bridgman crystals. The best dosimeters were made with silver chloride crystals containing 5 to 10 ppm of lead; other impurities tested did not produce proper dosimeters.

Childs, C. B.↗

Process for preparing higher oxides of the alkali and alkaline earth metals

High purity inorganic higher oxides of the alkali and alkaline earth metals are prepared by subjecting the hydroxide of the alkali and alkaline earth metal to a radio frequency discharge sustained in oxygen. The process is particulary adaptable to the production of high purity potassium superoxide by subjecting potassium hydroxide to glow discharge sustained in oxygen under the pressure of about 0.75 to 1.00 torr.

Sadhukhan, P.↗

Quality control during IC processing

Manual gives detailed test procedures for controlling silicon-wafer processing in manufacture of integrated circuits. Included among 43 test procedures are: ionic, bacterial, and solids contamination of high-purity water needed for wafer processing; crystallographic reflection, purity, and orientation; substrate dimensions and finish; thickness of deposited epitaxial films; oxide quality; photoresist characteristics; pinholes in insulating layers; metallized adhesion; and quality of ohmic contact.

Source record↗

Silicon halide-alkali metal flames as a source of solar grade silicon

The feasibility of using alkali metal-silicon halide diffusion flames to produce solar-grade silicon in large quantities and at low cost is demonstrated. Prior work shows that these flames are stable and that relatively high purity silicon can be produced using Na + SiCl4 flames. Silicon of similar purity is obtained from Na + SiF4 flames although yields are lower and product separation and collection are less thermochemically favored. Continuous separation of silicon from the byproduct alkali salt was demonstrated in a heated graphite reactor. The process was scaled up to reduce heat losses and to produce larger samples of silicon. Reagent delivery systems, scaled by a factor of 25, were built and operated at a production rate of 0.5 kg Si/h. Very rapid reactor heating rates are observed with wall temperatures reaching greater than 2000 K. Heat release parameters were measured using a cooled stainless steel reactor tube. A new reactor was designed.

Olsen, D. B.↗

Bubble behavior during solidification in low-gravity

The trapping and behavior of gas bubbles were studied during low gravity solidification of carbon tetrabromide. The flight experiments were performed during two sounding rocket flights (SPAR 1 and SPAR 3) and involved gradient freeze solidification of gas saturated melts. Gas bubbles were evolved at the solid-liquid interfaces during the low gravity intervals. No large-scale thermal migration of bubbles, bubble pushing by the solid-liquid interface, or bubble detachment from the interface were observed during the low gravity experiments. During the SPAR 3 experiment, a unique bubble motion-fluid flow event occurred in one specimen: a large bubble moved downward and caused some circulation of the melt. The gas bubbles that were trapped by the solid in commercial purity material formed voids that had a cyclindrical shape in SPAR 3, in contrast to the spherical shape that had been observed in SPAR 1. These shapes were not influenced by the gravity level, but were dependent upon the initial temperature gradient. In higher purity material the shape of the voids changed from cylindrical in one-g to spherical in low-g.

Papazian, J. M.↗

Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions

X-ray Photoelectron Spectroscopy (XPS) was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

Wheeler, D. R.↗

Electrodeposition applications for the Space Shuttle Main Engine

Electrodeposition processes play a key role in the fabrication and in-service performance of the Space Shuttle Main Engine. Applications range from the electroforming of the main combustion chamber to the deposition of high-purity copper or gold for hydrogen embrittlement protection of susceptible materials of construction, or nickel for mechanical protection of foam insulated propellant ducts. Techniques for controlling electrolyte purity, verification of deposit integrity, and deposit profile and thickness are reported. The use of in-situ techniques (cell-plating) for localized plating and repair of damaged substrate materials are summarized.

Otousa, J. E.↗

Synthesis of amino acyl adenylates using the tert-butoxycarbonyl protecting group

The synthesis of amino acyl adenylates using N-tert-butoxycarbonyl-protected amino acids is reported. Anhydrous solutions containing N-tert-butoxycarbonyl alanine, phenylalanine, and methionine were combined with the anhydrous mono (tri-n-octylammonium) salt of adenosine 5'-phosphate and the resultant amino acyl adenylates were characterized by means of elemental analysis, and infrared and proton NMR spectroscopy. Amino acyl adenylate yields of up to 60% were obtained with high purity at room temperatures. The reported synthesis is considered to represent a large improvement over previous methods due to the purity of the products, normal temperature requirements, and the stability of the starting compounds, which suggests its use in investigations of prebiotic oligo- and polypeptide synthesis.

Armstrong, D. W.↗