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Organosilicon polymers were synthesized to produce improved physical and chemical properties, including high thermal stability. Of the polymers produced, poly/4, 4 prime-bisoxybi- phenylene/diphenylsilane, formed from bis/anilino/diphenylsilane and p, p prime-biphenol, was found to have the most desirable properties.
Preparation of cross-linkable linear high molecular weight polyaryloxysilanes
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Fast He and Ar beams have been scattered by room-temperature CH4, SiH4, and GeH4 to obtain average atom-molecule potentials for He-CH4, He-SiH4, He-GeH4, Ar-CH4, and Ar-GeH4. Somewhat unexpectedly, the potential for He-GeH4 was intermediate between He-CH4 and He-SiH4; this apparent discrepancy, however, correlates with the bond polarities. The potential for Ar-CH4 can be satisfactorily predicted from that for He-CH4 by means of simple potential models and combination rules. The analogous prediction for Ar-GeH4 is unsatisfactory; reasons for the discrepancy are discussed.
The kinetics of the redistribution of dichlorosilane and trichlorosilane vapor over a tertiary amine ion exchange resin catalyst were investigated. The hydrogenation of SiCl4 to form HSiCl3 and the direct synthesis of H2SiCl2 from HCl gas and metallurgical silicon metal were also studied. The purification of SiH4 using activated carbon adsorbent was studied along with a process for storing SiH4 absorbed on carbon. The latter makes possible a higher volumetric efficiency than compressed gas storage. A mini-plant designed to produce ten pounds per day of SiH4 is described.
The feasibility of using a non-equilibrium hydrogen plasma jet as a chemical synthesis tool was investigated. Four possible processes were identified for further study: (1) production of polycrystalline silicon photovoltaic surfaces, (2) production of SiHCl3 from SiCl4, (3) production of SiH4 from SiHCl3, and (4) purification of SiCl4 by metal impurity nucleation. The most striking result was the recognition that the strongly adhering silicon films, amorphous or polycrystalline, produced in our studies could be the basis for preparing a photovoltaic surface directly; this process has potential advantages over other vapor deposition processes.
The design, fabrication, and installation of an experimental process system development unit (EPSDU) were analyzed. Supporting research and development were performed to provide an information data base usable for the EPSDU and for technological design and economical analysis for potential scale-up of the process. Iterative economic analyses were conducted for the estimated product cost for the production of semiconductor grade silicon in a facility capable of producing 1000-MT/Yr.
The results of the free space reactor experimental work are summarized. Overall, the objectives were achieved and the unit can be confidently scaled to the EPSDU size based on the experimental work and supporting theoretical analyses. The piping and instrumentation of the fluidized bed reactor was completed.
Detailed characterizaton and formulation studies were performed on a methyltriakoxysilane hydrolysate as a binder for thermal control coatings. The binder was optimized by varying hydrolysis temperature, time, catalyst type, and water concentration. The candidate coating formulations, based on this binder with TiO2 pigment, were optimized via a detailed series of sprayed test panels that included the parameters of binder/pigment ratio, ethanol content, pigment particle size, coating thickness and cure conditions. A typical optimized coating was prepared by acetic acid catalyzed hydrolysis of methyltriethoxysilane with 3.25 mol-equivalents of water over a 24 hour period at room temperature. The resulting hydrolysate was directly mixed with pre-milled TiO2 (12 grams pigment/26 grams binder) to yield a sprayable consistency. Panels were sprayed to result in a nominal cure coating thickness of 2 mils. Cure was affected by air drying for 24 hr at room temperature plus 72 hr at 150 F. These coatings are typically extremely tough and abrasion-resistant, with an absorptance (alpha) of 0.20 and emittance (e) of 0.89. No significant coating damage was observed in the mandrel bend test, even after exposure to thermal cycling from -160 to 160 F. Vacuum exposure of the coatings for 930 hours at 1 equivalent UV sun resulted in no visible degradation and no significant increase in absorptance.
Technical report describes theoretical and experimental development of methyltriethoxysilane (MTES) hydrolysate binder for white, titanium dioxidepigmented thermal-control coatings often needed on satellites. New coating is tougher and more abrasion-resistant than conventional coating, S-13G, which comprises zinc oxide in hydroxyl-therminated dimethylsiloxane binder.
The engineering design, fabrication, assembly, operation, economic analysis, and process support research and development for an Experimental Process System Development Unit for producing semiconductor-grade silicon using the slane-to-silicon process are reported. The design activity was completed. About 95% of purchased equipment was received. The draft of the operations manual was about 50% complete and the design of the free-space system continued. The system using silicon power transfer, melting, and shotting on a psuedocontinuous basis was demonstrated.
The engineering design, fabrication, assembly, operation, economic analysis, and process support R and D for an Experimental Process System Development Unit (EPSDU) are reported. About 95% of purchased equipment is received and will be reshipped to the West Coast location. The Data Collection System is completed. In the area of melting/consolidation, to the system using silicon powder transfer, melting and shotting on a pseudocontinuous basis is demonstrated. It is proposed to continue the very promising fluid bed work.
The use of selected organosilicon compounds for the preparation of silicon based ceramic materials is discussed in terms of processing microstructure-property relationships. The mechanisms operative in the formation of gel derived silicate glasses and glass ceramics are reasonably well understood, but this is not true for silicon carbide/nitride based ceramics. The properties of organosilicon precursors and the mechanism of pyrolysis affect the microstructural features of the ceramic. Reaction mechanisms are proposed and the microstructural features and properties of organosilazane derived ceramics discussed.
Scraper removes silicon deposits from inner walls of reactor vessel. Scraper supported by gas bearing. Scraper made of non-contaminating material such as quartz or silicon.
The process technology for the manufacture of semiconductor-grade silicon in a large commercial plant by 1986, at a price less than $14 per kilogram of silicon based on 1975 dollars is discussed. The engineering design, installation, checkout, and operation of an Experimental Process System Development unit was discussed. Quality control of scaling-up the process and an economic analysis of product and production costs are discussed.
Seed particles for fluidized-bed production of silicon made by new contamination-free, economical method. In new method, large particles of semiconductor-grade silicon fired at each other by high-speed streams of gas and thereby break up into particles of suitable size for fluidized bed. No foreign materials introduced, and leaching unnecessary. Method used to feed fluidized-bed reactor for continuous production of high-purity silicon.
In situ plasma diagnostics using coherent anti-Stokes Raman spectroscopy have shown different dissociation characteristics for GeH4 and SiH4 in radio frequency (rf) plasma-enhanced chemical vapor deposition of amorphous silicon germanium alloy (a-SiGe:H) thin films. The GeH4 dissociation rate in rf plasmas is a factor of about 3 larger than that of SiH4. Plasma diagnostics have revealed that the hydrogen dilution of the SiH4 and GeH4 mixed plasma plays a critical role in suppressing the gas phase polymerization and enhancing the GeH4 dissociation.
Highly photosensitive a-SiGe:H films with a light-to-dark conductivity ratio of 8 x 103 and an optical bandgap of 1.40 eV have been produced by RF glow discharge using hydrogen dilution of SiH4 and GeH4 mixed gas plasma. The critical role of hydrogen dilution in GeH4 containing plasmas is to suppress the gas-phase polymerization and promote the incorporation of Ge into the film. It is observed that inelastic laser light scattering of the RF plasma is a sensitive method for monitoring the onset of the gas-phase polymerization. In situ coherent anti-Stokes Raman spectroscopy measurements have shown that the dissociation rate of GeH4 is a factor of three larger than that of SiH4.