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At least 163 records · Page 9

Mass spectrometric studies of phosphine pyrolysis and OMVPE growth of InP

The mechanism of PH3 decomposition was studied by using D2 as a carrier gas and analyzing the reaction products with a mass spectrometer. The effects of InP and silica surfaces were investigated. The only gaseous product below 600 C is H2. Since any gas-phase H atoms would produce HD, the reaction occurs entirely on the surface. The slow step is the unimolecular removal of the first hydrogen atom, with an activation energy of 36.0 kcal/mole on InP surfaces. The reaction on InP is first-order for PH3 concentrations as high as 15 percent, so the surface is not saturated at those conditions. When trimethylindium (TMIn) is added to the gas mixture, the mechanism changes dramatically, probably proceeding via an unstable intermediate adduct of TMIn and PH3 which eliminates CH4 upon formation. This concerted reaction lowers the pyrolysis temperatures of both PH3 and TMIn.

Larsen, C. A.↗

Lignin Sensor Based On Flash-Pyrolysis Mass Spectrometry

New lignin sensor takes only few minutes to measure lignin content of specimen of wood, pulp, paper, or similar material. Includes flash pyrolizer and ion-trap detector that acts as mass spectrometer. Apparatus measures amount of molecular fragments of lignin in pyrolysis products of samples. Helpful in controlling digestors in paper mills to maintain required lignin content, and also in bleaching plants, where good control of bleaching becomes possible if quick determination of lignin content made.

Kwack, Eug Y.↗

Silane-Pyrolysis Reactor With Nonuniform Heating

Improved reactor serves as last stage in system processing metallurgical-grade silicon feedstock into silicon powder of ultrahigh purity. Silane pyrolized to silicon powder and hydrogen gas via homogeneous decomposition reaction in free space. Features set of individually adjustable electrical heaters and purge flow of hydrogen to improve control of pyrolysis conditions. Power supplied to each heater set in conjunction with flow in reactor to obtain desired distribution of temperature as function of position along reactor.

Iya, Sridhar K.↗

Soot formation in shock-tube pyrolysis and oxidation of vinylacetylene

Soot formation in vinylacetylene, and vinylacetylene-oxygen argon-diluted mixtures was studied behind reflected shock waves by monitoring the attenuation of a 632.8-nm He-Ne laser beam. The experiments were performed at temperatures of 1600-2500 K, pressures of 2.08-3.09 bar, and total carbon atom concentrations of (1.99-2.05) x 10 to the 17th atoms/cu cm. The experimental results obtained in pyrolysis of vinylacetylene are similar to those of acetylene, both in the order of magnitude of the soot yield and the shape of its temperature dependence. The addition of oxygen to vinylacetylene shifts the soot bell to lower temperature and, distinct from all other hydrocarbons studied in this laboratory, accelerates the production of soot with reaction time. The experimental results are interpreted in terms of possible chemical reaction.

Frenklach, M.↗

Evaluation of Kapton pyrolysis, arc tracking, and arc propagation on the Space Station Freedom (SSF) solar array Flexible Current Carrier (FCC)

Recent studies involving the use of polyimide Kapton coated wires indicate that if a momentary electrical short circuit occurs between two wires, sufficient heating of the Kapton can occur to thermally char (pyrolyze) the Kapton. Such charred Kapton has sufficient electrical conductivity to create an arc which tracks down the wires and possibly propagates to adjoining wires. These studies prompted an investigation to ascertain the likelihood of the Kapton pyrolysis, arc tracking and propagation phenomena, and the magnitude of destruction conceivably inflicted on Space Station Freedom's (SSF) Flexible Current Carrier (FCC) for the photovoltaic array. The geometric layout of the FCC, having a planar-type orientation as opposed to bundles, may reduce the probability of sustaining an arc. An experimental investigation was conducted to simulate conditions under which an arc can occur on the FCC of SSF, and the consequences of arc initiation.

Stueber, Thomas J.↗

Cyclopentadiene evolution during pyrolysis-gas chromatography of PMR polyimides

The effect of formulated molecular weight (FMW), extent of cure, and cumulative aging on the amount of cyclopentadiene (CPD) evolved from Polymerization of Monomeric Reactants (PMR) polyimides were investigated by pyrolysis-gas chromotography (PY-GC). The PMR polyimides are additional crosslinked resins formed from an aromatic diamine, a diester of an aromatic tetracarboxylic acid and a monoester of 5-norbornene-2, 3-dicarboxylic acid. The PY-GC results were related to the degree of crosslinking and to the thermo-oxidative stability (weight loss) of PMR polyimides. Thus, PY-GC has shown to be a valid technique for the characterization of PMR polyimide resins and composites via correlation of the CPD evolved versus the thermal history of the PMR sample.

Alston, William B.↗

Evaluation of Kapton pyrolysis, arc tracking, and arc propagation on the Space Station Freedom (SSF) solar array flexible current carrier (FCC)

Recent studies involving the use of polyimide Kapton coated wires indicate that if a momentary electrical short circuit occurs between two wires, sufficient heating of the Kapton can occur to themally chlar (pyrolyze) the Kapton. Such charred Kapton has sufficient electricxl conductivity to create an arc which tracks down the wires and possibly propagates to adjoining wires. These studies prompted an invetigation to ascertain the likelihood of Kapton pyrolysis, arc tracking and propagation phenomena, and the magnitude of destruction conceivably inflicted on Space Station Freedom's (SSF's) Flexible Current Carrier (FCC) for the photovoltaic array. The geometric layout of the FCC, having a planar-type orientation as opposed to bundles, may reduce the probability of sustaining an arc. An experimental investigation was conducted to simulate conditions under which an arc can occur on the FCC of the SSF, and the consequences of arc initiation.

Stueber, Thomas J.↗

Vapor phase pyrolysis

The vapor phase pyrolysis process is designed exclusively for the lunar production of oxygen. In this concept, granulated raw material (soil) that consists almost entirely of metal oxides is vaporized and the vapor is raised to a temperature where it dissociates into suboxides and free oxygen. Rapid cooling of the dissociated vapor to a discrete temperature causes condensation of the suboxides, while the oxygen remains essentially intact and can be collected downstream. The gas flow path and flow rate are maintained at an optimum level by control of the pressure differential between the vaporization region and the oxygen collection system with the aid of the environmental vacuum.

Steurer, Wolfgang↗

Evaluation of Kapton pyrolysis, arc tracking, and flashover on SiO(x)-coated polyimide insulated samples of flat flexible current carriers for Space Station Freedom

Kapton polyimide wiring insulation was found to be vulnerable to pyrolization, arc tracking, and flashover when momentary short-circuit arcs have occurred on aircraft power systems. Short-circuit arcs between wire pairs can pyrolize the polyimide resulting in a conductive char between conductors that may sustain the arc (arc tracking). Furthermore, the arc tracking may spread (flashover) to other wire pairs within a wire bundle. Polyimide Kapton will also be used as the insulating material for the flexible current carrier (FCC) of Space Station Freedom (SSF). The FCC, with conductors in a planar type geometric layout as opposed to bundles, is known to sustain arc tracking at proposed SSF power levels. Tests were conducted in a vacuum bell jar that was designed to conduct polyimide pyrolysis, arc tracking, and flashover studies on samples of SSF's FCC. Test results will be reported concerning the minimal power level needed to sustain arc tracking and the FCC susceptibility to flashover. Results of the FCC arc tracking tests indicate that only 22 volt amps were necessary to sustain arc tracking (proposed SSF power level is 400 watts). FCC flashover studies indicate that the flashover event is highly unlikely.

Stueber, Thomas J.↗

Model for the formation of silicon carbide from the pyrolysis of dichlorodimethylsilane in hydrogen. I - Silicon formation from chlorosilanes. II - Silicon carbide formation from silicon and methane

In the first part of this work, a model is developed for the deposition of silicon from the reduction of silicon tetrachloride with hydrogen in a tubular reactor at 700-1100 C, at atmospheric pressure. The model is based on gas chromatography of the volatile products of the reaction, followed by gravimetric analysis of total Si deposition on the tube. In the second part of this work, a model is developed for the case of SiC deposition from the pyrolysis of dichlorodimethylsilane in hydrogen under the same reactor conditions. The rate constants derived from a nonlinear regression analysis are reported.

Cagliostro, Domenick E.↗

Thermal History Of PMRs Via Pyrolysis-Gas Chromatography

Pyrolysis-gas chromatography (PY-GC) useful as analytical technique to determine extents of cure or postcure of PMR-15 polyimides and to lesser extent, cumulative thermal histories of PMR-15 polyimides exposed to high temperatures. Also applicable for same purposes to other PMR polyimides and to composite materials containing PMR polyimides. Valuable in reducing costs and promoting safety in aircraft industry by helping to identify improperly cured or postcured PMR-15 composite engine and airframe components and helping to identify composite parts nearing ends of their useful lives.

Gluyas, Richard E.↗

Mass spectrometer-pyrolysis experiment for atmospheric and soil sample analysis on the surface of Mars

Results from the Viking mission will form the foundation for future in-depth investigations of atmosphere-surface interactions on Mars. The two Viking landers carried impressive instrumentation to obtain and analyze soil samples: the sites were observed by cameras, and the collector head was located on a long boom and allowed the collection of large samples at various depths. A selection of grain sizes was possible and a distribution system supplied a number of experiments with soil material. Despite stationary vehicles, a wide sampling field was reachable. The GCMS system, responsible for atmospheric as well as surface soil analysis, worked well on both landers. Atmospheric measurements resulted in the determination of the abundance of noble gases as well as of other molecular species. Isotopic composition measurements included the important ratios of C-13/C-12, N-15/N-14, and Ar-36/Ar-40. To verify these past results and to advance detailed studies of noble gas isotope ratios and minor constituents, better instrument sensitivities, higher precision, and lower background contributions are required in future Mars missions. Soil analysis during the Viking mission concentrated on organic material. Heating cycles were performed to 500 C and only water and carbon dioxide were identified. Higher pyrolysis temperatures are of primary importance to advance our understanding of the mineralogy and gas loading of surface material and atmospheric exchange.

Mauersberger, Konrad↗

Coupled Ablation, Heat Conduction, Pyrolysis, Shape Change and Spallation of the Galileo Probe

The Galileo probe enters the atmosphere of Jupiter in December 1995. This paper presents numerical methodology and detailed results of our final pre-impact calculations for the heat shield response. The calculations are performed using a highly modified version of a viscous shock layer code with massive radiation coupled with a surface thermochemical ablation and spallation model and with the transient in-depth thermal response of the charring and ablating heat shield. The flowfield is quasi-steady along the trajectory, but the heat shield thermal response is dynamic. Each surface node of the VSL grid is coupled with a one-dimensional thermal response calculation. The thermal solver includes heat conduction, pyrolysis, and grid movement owing to surface recession. Initial conditions for the heat shield temperature and density were obtained from the high altitude rarefied-flow calculations of Haas and Milos. Galileo probe surface temperature, shape, mass flux, and element flux are all determined as functions of time along the trajectory with spallation varied parametrically. The calculations also estimate the in-depth density and temperature profiles for the heat shield. All this information is required to determine the time-dependent vehicle mass and drag coefficient which are necessary inputs for the atmospheric reconstruction experiment on board the probe.

Milos, Frank S.↗

Thin Film CuInS2 Prepared by Spray Pyrolysis with Single-Source Precursors

Both horizontal hot-wall and vertical cold-wall atmospheric chemical spray pyrolysis processes deposited near single-phase stoichiometric CuInS2 thin films. Single-source precursors developed for ternary chalcopyrite materials were used for this study, and a new liquid phase single-source precursor was tested with a vertical cold-wall reactor. The depositions were carried out under an argon atmosphere, and the substrate temperature was kept at 400 C. Columnar grain structure was obtained with vapor deposition, and the granular structure was obtained with (liquid) droplet deposition. Conductive films were deposited with planar electrical resistivities ranging from 1 to 30 Omega x cm.

Jin, Michael H.↗

The Effect of Film Composition on the Texture and Grain Size of CuInS2 Prepared by Spray Pyrolysis

CuInS2 was deposited by spray pyrolysis using single-source precursors synthesized in-house. Films with either (112) or (204/220) preferred orientation always showed Cu-rich and In-rich composition respectively. The In-rich (204/220)-oriented films always contained a secondary phase evaluated as an In-rich compound, and the hindrance of (112)-oriented grain growth was confirmed by glancing angle X-ray diffraction. In conclusion, only the Cu-rich (112)-oriented films with dense columnar grains can be prepared without the secondary In-rich compound. The effect of extra Cu on the grain size and the solar cell results will be also presented.

Jin, Michael H.-C.↗

The Effect of Film Composition on the Texture and Grain Size of CuInS2 Prepared by Spray Pyrolysis

Ternary single-source precursors were used to deposit CuInS2 thin films using chemical spray pyrolysis. We investigated the effect of the film composition on texture, secondary phase formation, and grain size. As-grown films were most often In-rich. They became more (204/220)-oriented as indium concentration increased, and always contained a yet unidentified secondary phase. The (112)-prefened orientation became more pronounced as the film composition became more Cu-rich. The secondary phase was determined to be an In-rich compound based on composition analysis and Raman spectroscopy. In addition, as-grown Cu-rich (112)-oriented films did not exhibit the In-rich compound. Depositing a thin Cu layer prior to the growth of CuInS2 increased the maximum grain size from - 0.5 micron to - 1 micron, and prevented the formation of the In-rich secondary phase.

Jin, Michael H.↗

Detecting Pyrolysis Products from Bacteria in a Mars Soil Analogue

One of the primary objectives of the 1976 Viking missions was to determine whether organic compounds, possibly of biological origin, were present in the Martian surface soils. The Viking gas chromatography mass spectrometry (GCMS) instruments found no evidence for any organic compounds of Martian origin above a few parts per billion in the upper 10 cm of surface soil, suggesting the absence of a widely distributed Martian biota. However, it is now known that key organic compounds important to biology, such as amino acids, carboxylic acids and nucleobases, would likely have been missed by the Viking GCMS instruments. In this study, a Mars soil analogue that was inoculated with approx. 10 billion Escherichia coli cells was heated at 500 C under Martian ambient pressure to release volatile organic compounds from the sample. The pyrolysis products were then analyzed for amino acids and nucleobases using high performance liquid chromatography (HPLC) and GCMS. Our experimental results indicate that at the part per billion level, the degradation products generated from several million bacterial cells per gram of Martian soil would not have been detected by the Viking GCMS instruments. Upcoming strategies for Mars exploration will require in-situ analyses by instruments that can assess whether any organic compounds, especially those that might be associated with life, are present in Martian surface samples.

Glavin, D. P.↗