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Report lists tables of standard free-energy change, equilibrium constant, and heat of reaction for chemical vapor deposition (CVD) of silicon from silane over temperature range of 100 to 1000 K. Data indicates silicon CVD may be a commercially economical process for production of silicon for solar arrays and other applications.
The original objective of this program was to determine the feasibility of high volume, low-cost production of high purity silane or solar cell grade silicon using a non equilibrium plasma jet. The emphasis was changed near the end of the program to determine the feasibility of preparing photovoltaic amorphous silicon films directly using this method. The non equilibrium plasma jet should be further evaluated as a technique for producing high efficiency photovoltaic amorphous silicon films.
The feasibility of Union Carbide's silane process for commercial application was established. An integrated process design for an experimental process system development unit and a commercial facility were developed. The corresponding commercial plant economic performance was then estimated.
This phase consists of the engineering design, fabrication, assembly, operation, economic analysis, and process support R&D for an Experimental Process System Development Unit (EPSDU). The mechanical bid package was issued and the bid responses are under evaluation. Similarly, the electrical bid package was issued, however, responses are not yet due. The majority of all equipment is on order or has been received at the EPSDU site. The pyrolysis/consolidation process design package was issued. Preparation of process and instrumentation diagram for the free-space reactor was started. In the area of melting/consolidation, Kayex successfully melted chunk silicon and have produced silicon shot. The free-space reactor powder was successfully transported pneumatically from a storage bin to the auger feeder twenty-five feet up and was melted. The fluid-bed PDU has successfully operated at silane feed concentrations up to 21%. The writing of the operating manual has started. Overall, the design phase is nearing completion.
Melter directly coupled to pyrolyzer eliminates difficulties of transport. Proposed coupling of free-space silane pyrolyzer and melter without intervening steps produce molten silicon with no problems of fine-particle movement, storage, contamination in transport, or oxide formation.
The ion-molecule and radical-molecule mechanisms are responsible for the dissociation of hydrocarbon, silane, and chlorosilane monomers and the formation of polymerized species, respectively, in an RF plasma discharge. In a plasma containing a mixture of monomer and argon the rate-determining step for both dissociation and polymerization is governed by an ion-molecule type of interaction. Adding hydrogen or ammonia to the monomer-argon mixture transforms the rate-determining step from an ion-molecule interaction to a radical-molecule interaction for both monomer dissociation and polymerization.
Technical activities are reported in the design of process, facilities, and equipment for producing silicon at a rate and price comensurate with production goals for low cost solar cell modules. The silane-silicone process has potential for providing high purity poly-silicon on a commercial scale at a price of fourteen dollars per kilogram by 1986, (1980 dollars). Commercial process, economic analysis, process support research and development, and quality control are discussed.
Silane has been detected in the gas surrounding IRC +10216. Thirteen absorption lines in the nu-4 band around 917/cm were observed at 0.2 km/s resolution. A lower limit to the radial column density is 2 x 10 to the 15th/sq cm, and the relative strengths of the transitions indicate an average rotational temperature of 173 K.
A chemical kinetic mechanism is proposed for the combustion of silane-hydrogen-oxygen-nitrogen mixtures in the initial temperature range from 800K to 1250K and pressure range from 0.5 to 1.35 atm. The mechanism yields results which are in agreement with published ignition delay times obtained from shock tube experiments. Comparisons between the results obtained using the proposed mechanism and that of an alternative mechanism reveal that the former predicts appreciably shorter ignition delay times, but a flame blowout envelope which is shifted so as to decrease the stable flame region. Over much of the thermodynamic range examined, the mechanism predicts long reaction times. A three step global mechanism is proposed which closely models the ignition phase of SiH4 - H2 - air combustion; however, the reaction phase is less well reproduced by the global model. The necessity for additional experimental data to further assess the proposed models is stressed.
Concluding tests for the thermogravimetric and FTIR analyses of DC 1200 silane primers are discussed as well as methods for HPLC and GC analyses and for determining titanium and silicon by atomic absorption spectroscopy. Tables summarizes results obtained for residue, ash, titanium, silicone, Si/Ti ratio, OH-absorption, the lap-shear test, and the GC headspace for alcohols.
Results of lap shear tests of various silane primers are presented in graphs and tables. The OH-absorption of these primers (FTIR area values) are correlated with the lap shear tests of coated panels.
The silane decomposition in a fluidized bed reactor was studied. The process feasibility and operating windows were determined. Long duration tests were conducted and silicon purity was demonstrated. A high purity linear was installed in the fluid bed reactor; the FBR product was melted and single crystallized. Product purity improvements are noted.
Development of a mathematical model for fluidized bed pyrolysis of silane that relates production rate and product properties (size, size distribution, presence or absence of fines) with bed size and operating conditions (temperature, feed concentration, flow rate, seed size, etc.) and development of user oriented algorithm for the model are considered. A parameter sensitivity study of the model was also developed.
Silane-endcapped polyimide high temperature adhesive formulations were prepared by reacting anhydride-terminated poly(amic acid), obtained from benzophenonetetracarboxylic dianhydride and a diamine (3,3'-, 3,4'- or 4,4'-diaminodiphenylmethane and 3,3', 3,4'- or 4,4'-diaminobenzophenone) with varying amounts of gama-aminopropyltriethoxysilane in dimethylacetamide. Resin properties were evaluated by torsional braid analysis and thermogravimetric analysis. Lap shear strengths of some of the adhesive bonds were determined at room temperature and at 177 C before and after ageing at 200 C for 2500 h and after boiling in water for 72 h.
Costly gas purified after use in deposition reactor. Proposed method for recycling silane reduces cost of producing pure silicon for semiconductor devices.
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.
A new visualization technique for reacting flows has been developed. This technique, which is suitable for supersonic combustion flows, has been demonstrated on a scramjet combustor model. In this application, gaseous silane (SiH4) was added to the primary hydrogen fuel. When the fuel reacted, so did the (SiH4), producing silica (SiO2) particles in situ. The particles were illuminated with a laser sheet formed from a frequency-doubled Nd:YAG laser (532 nm) beam and the Mie scattering signal was imaged. These planar images of the silica Mie scattering provided instantaneous 'maps' of combustion progress within the turbulent reacting flowfield.
The size of the agglomerates produced in the upper portion of a flame is important for a variety of applications. Soot particle size and density effect the amount of radiative heat transfer from a fire to its surroundings. Particle size determines the lifetime of smoke in a building or in the atmosphere, and exposure hazard for smoke inhaled and deposited in the lungs. The visibility through a smoke layer and dectectability of the smoke are also greatly affected by agglomerate size. Currently there is limited understanding of soot growth with an overall dimension of 10 m and larger. In the case of polystyrene, smoke agglomerates in excess of 1 mm have been observed raining out from large fires. Unlike hydrocarbon fuels, silane has the advantage that silica particles are the major combustion product resulting in a particle volume fraction a factor of ten greater than that for a carbonaceous smoke. There are two very desirable properties of silica aero-gels that are important for both space and earth based applications. The first important property is its inertness to most oxidizing and reducing atmospheres. Therefore, silica aero-gels make excellent fire ablatives and can be used in very demanding applications. The second important property is that silica aero-gels are expected to have very high porosity (greater than 0.999), making them lightweight and ideal for aerospace applications. The added benefit of the high porosity is that they can be used as extremely efficient filters for many earth based applications as well. Evidence of the formation of superagglomerates in a laminar acetylene/air diffusion flame was found by Sorensen et al. [1]. An interconnecting web of super-agglomerates was observed to span the width of the soot plume in the region just above the flame tip and described as a gel state. It was observed that this gel state immediately breaks up into agglomerates as larges as 100 m due to buoyancy induced turbulence. Large soot agglomerates were observed in microgravity butane jet diffusion flames by Ito et al.[2]. Several other works to date have studied the effect of flame structure on soot volume fraction and agglomeration size in a microgravity environment.[3-4]. In microgravity the absence of buoyant convective flows increases the residence time in the flame and causes a broadening of the high temperature region in the flame. Both of these factors play a significant role in gas phase radiation and soot formation