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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1978

Low cost silicon solar array project: Feasibility of low-cost, high-volume production of silane and pyrolysis of silane to semiconductor-grade silicon

Silicon epitaxy analysis of silane produced in the Process Development Unit operating in a completely integrated mode consuming only hydrogen and metallurgical silicon resulted in film resistivities of up to 120 ohms cm N type. Preliminary kinetic studies of dichlorosilane disproportionation in the liquid phase have shown that 11.59% SiH4 is formed at equilibrium after 12 minutes contact time at 56 C. The fluid-bed reactor was operated continuously for 48 hours with a mixture of one percent silane in helium as the fluidizing gas. A high silane pyrolysis efficiency was obtained without the generation of excessive fines. Gas flow conditions near the base of the reactor were unfavorable for maintaining a bubbling bed with good heat transfer characteristics. Consequently, a porous agglomerate formed in the lower portion of the reactor. Dense coherent plating was obtained on the silicon seed particles which had remained fluidizied throughout the experiment.

Breneman, W. C.↗
NASA NTRS1977

Low cost silicon solar array project silicon materials task: Establishment of the feasibility of a process capable of low-cost, high volume production of silane (step 1) and the pyrolysis of silane to semiconductor-grade silicon (step 2)

Extended operation of a small process-development unit routinely produced high quality silane in 97+% yield from dichlorosilane. The production rate was consistent with design loadings for the fractionating column and for the redistribution reactor. A glass fluid-bed reactor was constructed for room temperature operation. The behavior of a bed of silcon particles was observed as a function of various feedstocks, component configurations, and operating conditions. For operating modes other than spouting, the bed behaved in an erratic and unstable manner. A method was developed for casting molten silicon powder into crack-free solid pellets for process evaluation. The silicon powder was melted and cast into thin walled quartz tubes that sacrificially broke on cooling.

Breneman, W. C.↗
NASA NTRS1977

Low cost silicon solar array project silicon materials task: Establishment of the feasibility of a process capable of low-cost, high volume production of silane (step 1) and the pyrolysis of silane to semiconductor-grade silicon (step 2)

A quartz fluid bed reactor capable of operating at temperatures of up to 1000 C was designed, constructed, and successfully operated. During a 30 minute experiment, silane was decomposed within the reactor with no pyrolysis occurring on the reactor wall or on the gas injection system. A hammer mill/roller-crusher system appeared to be the most practical method for producing seed material from bulk silicon. No measurable impurities were detected in the silicon powder produced by the free space reactor, using the cathode layer emission spectroscopic technique. Impurity concentration followed by emission spectroscopic examination of the residue indicated a total impurity level of 2 micrograms/gram. A pellet cast from this powder had an electrical resistivity of 35 to 45 ohm-cm and P-type conductivity.

Breneman, W. C.↗
NASA NTRS1986

Opposed jet burner studies of silane-methane, silane-hydrogen and hydrogen diffusion flames with air

An atmospheric pressure tubular opposed jet burner technique was used to characterize certain diffusion-flame transitions and associated burning rates for N2-diluted mixtures of highly-reactive fuels. Presented are: (1) details of the technique, with emphasis on features permitting the study of flames involving pyrophoric gases and particle-forming combustion reactions: (2) discoveries on the properties of these flames which correspond to physically and chemically distinct stages of silane and hydrogen combustion; and (3) unburnt gas velocity data obtained from flames based on SiH4-CH4-N2, SiH4-H2-N2, and H2-N2 fuel mixtures, and plotted as functions of combustible-fuel mole fraction and fuel/oxygen molar input flow ratios. In addition, these burning velocity results are analyzed and interpreted.

Pellett, G. L.↗
NASA NTRS1986

Opposed jet burner studies of silane-methane, silane-hydrogen, and hydrogen diffusion flames with air

An atmospheric pressure tubular opposed jet burner technique was used to characterize certain diffusion-flame transitions and associated burning rates for N2-diluted mixtures of highly-reactive fuels. The paper presents: (1) details of the technique, with emphasis on features permitting the study of flames involving pyrophoric gases and particle-forming combustion reactions; (2) discoveries on the properties of these flames which correspond to physically and chemically distinct stages of silane and hydrogen combustion; and (3) unburnt gas velocity data obtained from flames based on SiH4-CH4-N2, SiH4-H2-N2, and H2-N2 fuel mixtures, and plotted as functions of combustible-fuel mole fraction and fuel/oxygen molar input flow ratios. In addition, these burning velocity results are analyzed and interpreted.

Pellett, G. L.↗
NASA NTRS1978

Low Cost Silicon Solar Array Project. Feasibility of Low-cost, High-volume Production of Silane and Pyrolysis of Silane to Semiconductor-grade Silicon

The presence of copper promotes a more rapid approach to the steady stete operating condition and results in a more consistent reactor effluent composition. The average kinetic and equilibrium yield are unchanged. Incoloy has been identified as the preferred choice of material of construction for the hydrogenation reactor although certain metallurgical changes were noted in samples exposed to the H2/HCl atmosphere at 500 C which indicate the need for more testing.

Breneman, W. C.↗
NASA NTRS2001

Organic-Inorganic Hybrids Using Novel Phenylethynyl Imide Silanes

In this presentation, polyimide-silica hybrids using novel phenylethynyl imide silanes are reported. The phenylethynyl group is present in the organic precursor as either a pendent or an end group to bond chemically with the polyimide adhesive containing phenylethynyl groups during processing, while the silane group of the organic precursor would chemically react with the inorganic precursor through oxane bond formation. The chemical compositions of these novel hybrids were examined using X-ray mapping modes of scanning electron microscopy (SEM), which revealed a silicon gradient interphase between the high surface energy substrate and the polyimide adhesive. Novel aromatic phenylethynyl imide silanes (APEISs) and pendent phenylethynyl imide oligomeric disilanes (PPEIDSs) have been synthesized, and sol-gel solutions containing the new silanes, a phenylethynyl terminated imide oligomer (PETI-5), and an inorganic precursor were formulated to develop a gradient hybrid interphase between a titanium alloy and the adhesive. Two different sol-gel systems were investigated to develop organic-inorganic hybrids. Hybrid I was composed of an organic precursor containing both phenylethynyl and silane groups (PPEIDS) and an inorganic precursor. Functional group concentrations were controlled by the variation of the molecular weight of the imide backbone of PPEIDS. Hybrid II was composed of organic and inorganic precursors and a coupling agent containing both phenylethynyl and silane groups. Morphology and chemical composition of the hybrid interphase between the inorganic substrate and the adhesive were investigated, and the bond strength and durability were evaluated using lap shear tests at various conditions. The assessment of how the bonding at an interface is affected by various sol-gel solution compositions and environments is reported.

Park, C.↗
NASA NTRS1986

Effect of silane concentration on the supersonic combustion of a silane/methane mixture

A series of direct connect combustor tests was conducted to determine the effect of silane concentration on the supersonic combustion characteristics of silane/methane mixtures. Shock tube ignition delay data indicated more than an order of magnitude reduction in ignition delay times for both 10 and 20 percent silane/methane mixtures as compared to methane. The ignition delay time of the 10 percent mixture was only a factor of 2.3 greater than that of the 20 percent mixture. Supersonic combustion tests were conducted with the fuel injected into a model scramjet combustor. The combustor was mounted at the exit of a Mach 2 nozzle and a hydrogen fired heater was used to provide a variation in test gas total temperature. Tests using the 20 percent silane/methane mixture indicated considerable combustion enhancement when compared to methane alone. This mixture had an autoignition total temperature of 1650 R. This autoignition temperature can be contrasted with 2330 R for hydrogen and 1350 R for a 20 percent silane/hydrogen mixture in similar hardware. Methane without the silane additive did not autoignite in this configuration at total temperatures as high as 3900 R, the maximum temperature at which tests were conducted. Supersonic combustion tests with the silane concentration reduced to 10 percent indicated little improvement in combustion performance over pure methane. The addition of 20 percent silane to methane resulted in a pyrophoric fuel with good supersonic combustion performance. Reducing the silane concentration below this level, however, yielded a less pyrophoric fuel that exhibited poor supersonic combustion performance.

Northam, G. B.↗
NASA NTRS1984

Measuring Trace Hydrocarbons in Silanes

Technique rapid and uses standard analytical equipment. Silane gas containing traces of hydrocarbons injected into carrier gas of moist nitrogen having about 0.2 percent water vapor. Carrier, water and silane pass through short column packed with powdered sodium hydroxide which combines moisture and silane to form nonvolatile sodium silicate. Carrier gas free of silane but containing nonreactive hydrocarbons, pass to silica-gel column where chromatographic separation takes place. Hydrocarbons measured by FID.

Lesser, L. A.↗
NASA NTRS1984

Fines in fluidized bed silane pyrolysis

Silicon deposition on silicon seed particles by silane pyrolysis in a fluidized-bed reactor is investigated as a low-cost, high-throughput method to produce high-purity polysilicon for solar-cell applications. Studies of fines, particles 0.1-10 microns diam, initiated from homogeneous decomposition in the reactor were conducted using 2 and 6-in-diam fluidized beds. The studies show functional dependences of fines elutriation on silane feed concentration, temperature, gas velocity, and bubble size. The observation that the fines elutriation is generally below 10 percent of the silicon-in-silane feed is attributed to scavenging by large particles in an environment of less free space for homogeneous nucleation. Preliminary results suggest that, with proper conditions and distributor design, high-silane-concentration (over 50 percent SiH4 in H2) feed may be used.

Hsu, G.↗
NASA NTRS1986

Development of the silane process for the production of low-cost polysilicon

It was recognized that the traditional hot rod type deposition process for decomposing silane is energy intensive, and a different approach for converting silane to silicon was chosen. A 1200 metric tons/year capacity commercial plant was constructed in Moses Lake, Washington. A fluidized bed processor was chosen as the most promising technology and several encouraging test runs were conducted. This technology continues to be very promising in producing low cost polysilicon. The Union Carbide silane process and the research development on the fluidized bed silane decomposition are discussed.

Iya, S. K.↗
NASA NTRS1987

In situ process diagnostics of silane plasma for device-quality a-Si:H deposition

Coherent anti-Stokes Raman spectroscopy (CARS) and mass spectrometry (MS) have been applied to in situ process diagnostics of a silane plasma for device-quality a-Si:H film deposition. Silane depletion was directly measured by CARS and is linearly dependent on RF power in the region of 4-12 W with a slope of 0.5 percent/mW-sq cm. The depletion is also dependent on SiH4 flow rate starting with a 50 percent depletion at a low flow rate of 5.6 sccm and asymptotically approaching an 8 percent depletion at a flow rate of 80 sccm. The mass spectral line signal intensity of disilane increases with RF power and shows an apparent transition at 6 W. Disilane formation in silane plasma, film deposition rate, and silane depletion ratio as a function of the RF power indicate that the film growth mechanism in the low-power region of 3.5-6.5 W is substantially different from that in the high-power region of 6.5-12 W.

Shing, Y. H.↗
NASA NTRS2002

Solid State Electrolytes Prepared from PEO (360) Silanated Silica

All solid state composite electrolytes were prepared using fumed silica (SiO2) silanated with an oligomeric polyethylene oxide (PEO) silane containing 6-9 ethylene oxide repeat units, a PEO matrix and LiClO4 (8/1 O/Li). The PEO-silane covalently attached to the silica was amorphous, with a T(sub g) that increased from -90 C to -53 C after attachment. The conductivity of films prepared using the PEO-silanated silica increased to approx. 6 x 10(exp -5) S/cm at RT compared with approx. 1 x 10(-5) S/cm for films prepared with unsilanated SiO2.

Maitra, P.↗
NASA NTRS1987

Zone heating for fluidized bed silane pyrolysis

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower reaction zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

Iya, Sridhar K.↗
NASA NTRS1989

Reactor for fluidized bed silane decomposition

An improved heated fluidized bed reactor and method for the production of high purity polycrystalline silicon by silane pyrolysis wherein silicon seed particles are heated in an upper heating zone of the reactor and admixed with particles in a lower zone, in which zone a silane-containing gas stream, having passed through a lower cooled gas distribution zone not conducive to silane pyrolysis, contacts the heated seed particles whereon the silane is heterogeneously reduced to silicon.

Iya, Sridhar K.↗
NASA NTRS1977

Chemical Vapor Deposition of Silicon from Silane Pyrolysis

The four basic elements in the chemical vapor deposition (CVD) of silicon from silane are analytically treated from a kinetic standpoint. These elements are mass transport of silane, pyrolysis of silane, nucleation of silicon, and silicon crystal growth. Rate expressions that describe the various steps involved in the chemical vapor deposition of silicon were derived from elementary principles. Applications of the rate expressions for modeling and simulation of the silicon CVD are discussed.

Praturi, A. K.↗
NASA NTRS1981

Silane pyrolysis in a free-space reactor

The Union Carbide process for producing silicon for photovoltaic applications proceeds via high purity silane as an intermediate. Decomposition of silane is accomplished in a freespace reactor which utilizes recirculating product hydrogen and silicon to transfer energy from a heated wall to an entering silane jet. Reaction occurs away from the wall, minimizing problems with wall deposition and contamination. A series of long duration and throughput tests has proven the feasibility of this concept. High purity powder can be produced at flows up to 4.5 kg/hr (10 lb/hr) in a 0.2 m (8 inch) diameter reactor with better than 99.99% conversion efficiency. This work is funded by DOE under JPL's Low Cost Solar Array (LSA) program.

Lay, J. R.↗
NASA NTRS1984

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

Silane primers for use as thermal protection on external tanks were subjected to various analytic techniques to determine the most effective testing method for silane lot evaluation. The analytic methods included high performance liquid chromatography, gas chromatography, thermogravimetry (TGA), and fourier transform infrared spectroscopy (FTIR). It is suggested that FTIR be used as the method for silane lot evaluation. Chromatograms, TGA profiles, bar graphs showing IR absorbances, and FTIR spectra are presented.

Mikes, F.↗