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Ultra-high-purity silicon required for solar cells, transistors and integrated circuits can be produced from metallurgical grade silicon by formation and pyrolysis of silane gas in continuous-flow process that maximizes product purity with minimum amount of equipment. Integrated process recycles unreacted and byproduct materials, minimizing material losses and simplifying waste disposal. Ensures effective removal of impurities, including boron.
Packed-bed reactor produces silicon by decomposing ultrapure silane gas in temperature gradient. Based on previous experiments with relatively low decomposition temperatures and with temperature gradients, heterogeneous decomposition will produce few fines. Fines produced are screened out and reinserted into furnace.
The interfacial chemistry of CVD SiO2 films deposited on thin native oxides grown on InSb substrates is examined using X-ray photoemission spectroscopy (XPS) and a relatively benign chemical etching technique for depth profiling. An intensity analysis of XPS spectra is used to derive the compositional structure of the interfaces obtained in the SiO2/native oxide/InSb system. Peak positions in these spectra are used to follow the change in substrate surface potential during the etch sequence, and to establish the chemical nature of the species formed during deposition and subsequent processing. Reaction of the substrate with oxygen resulted in an In-rich native oxide and 1-2 monolayers of excess elemental Sb at the native-oxide/substrate interface, incompletely oxidized silane reduced the native oxide, leaving less than 1 monolayer of elemental In at the SiO2/native oxide interface. Etch removal of this thin In-rich layer leads to a change in the substrate surface potential of 0.06 eV, corresponding to a net increase in positive charge. The results are consistent with simple thermodynamic considerations; they are also compared to previously reported studies of deposited dielectrics on III-V compound semiconductors.
Silane decomposition in a fluidized-bed reactor (FBR) process development unit (PDU) to make semiconductor-grade Si is reviewed. The PDU was modified by installation of a new heating system to provide the required temperature profile and better control, and testing was resumed. A process for making trichlorosilane by the hydrochlorination of metallurgical-grade Si and silicon tetrachloride is reported. Fabrication and installation of the test system employing a new 2-in.-dia reactor was completed. A process that converts trichlorosilane to dichlorosilane (DCS), which is reduced by hydrogen to make Si by a chemical vapor deposition step in a Siemens-type reactor is described. Testing of the DCS PDU integraled with Si deposition reactors continued. Experiments in a 2-in.-dia reactor to define the operating window and to investigate the Si deposition kinetics were completed.
Three different chemical processing schemes were identified for separating lunar soils into the major oxides and elements. Feedstock production for space industry; an HF acid leach process; electrorefining processes for lunar free metal and metal derived from chemical processing of lunar soils; production and use of silanes and spectrally selective materials; glass, ceramics, and electrochemistry workshops; and an econometric model of bootstrapping space industry are discussed.
A chemical kinetic reaction mechanism for the oxidation of silane/hydrogen mixtures is presented and discussed. Shock-tube ignition delay time data were used to evaluate and refine the mechanism. Good agreement between experimental results and the results predicted by the mechanism was obtained by adjusting the rate coefficient for the reaction SiH3 + O2 yields SiH2O + OH. The reaction mechanism was used to theoretically investigate the ignition characteristics of silane/hydrogen mixtures. The results revealed that over the entire range of temperature examined (800 K to 1200 K), substantial reduction in ignition delay times is obtained when silane is added to hydrogen.
Earlier studies have indicated that expenditures related to the preparation of high-purity silicon and its conversion to silicon sheet represent from 40 to 52 percent of the cost of the entire panel. The present investigation is concerned with the elements which were selected for study in connection with the Flat-Plate Solar Array (FSA) Project. The first of two technologies which are being developed within the FSA Project involves the conversion of metallurgical-grade silicon through a silane purification process to silicon particles. The second is concerned with the conversion of trichlorosilane to dichlorosilane, and the subsequent production of silicon using modified rod reactors of the Siemens type. With respect to silicon sheet preparation, efforts have been focused both on the preparation of ingots, followed by wafering, and the direct crystallization of molten silicon into a ribbon or film.
Silphenylene-siloxane polymers can be prepared by a condensation reaction of a diol 1,4-bis(hydroxydimethylsilyl)benzene and a silane bis(dimethylamino)dimethylsilane. Using a stepwise condensation technique, a polymer (R=CH3) with a molecular weight in excess of 1.0 x 1 million has been produced. The polymer exhibits increased thermal stability, compared to a methyl siloxane polymer without the aromatic phenyl ring in the backbone. The use of bis(dimethylamino)methylvinylsilane should allow for ready crosslinking at the vinyl sites (R=-CH=CH2) introduced into the backbone. However, under the conditions of the reaction system a high molecular weight polymer was not obtained or the polymer underwent a crosslinking process during the synthesis.
The use of silane (SiH4) as an effective ignitor and flame stabilizing pilot fuel is well documented. A reliable chemical kinetic mechanism for prediction of its behavior at the conditions encountered in the combustor of a SCRAMJET engine was calculated. The effects of hydrogen addition on hydrocarbon ignition and flame stabilization as a means for reduction of lengthy ignition delays and reaction times were studied. The ranges of applicability of chemical kinetic models of hydrogen-air combustors were also investigated. The CHARNAL computer code was applied to the turbulent reaction rate modeling.
MY-720/DDS epoxy samples were treated with three selected chemical compounds to render the active H-sites inactive for moisture absorption. Treating the epoxy castings with acetyl chloride and dichlorodimethyl silane leads only to surface changes indicating that these molecules are too large to penetrate the epoxy castings. Boron trifluoride, on the other hand, does penetrate the epoxy chain as is indicated by the formation of green domains in the interior of the castings. However, the process of saturating the specimens with moisture appears to leach out the chemical additives--thereby nullifying their possible ameliorative effects.
The preparation of very pure silicon from silane (SIH4) using radiant heating of the hot silicon particles of a fluidized bed is discussed. The fraction of electrical energy supplied to the heater which is actually absorbed by the particles and the heat transfer coefficient between the hot bed and the cool distributor plate were investigated. The experimental design is presented and the results of the study are summarized.
Tests for chemical structure, material properties, water absorption, aging and curing agent of Ethylene Vinyl Acetate (EVA) and UV absorption studies are carried out. A computer model was developed for thermal optical modeling, to investigate dependence between module operating temperature and solar insolation, and heat dissapation behavior. Structural analyses were performed in order to determine the stress distribution under wind and heat conditions. Curves are shown for thermal loading conditions. An electrical isolation was carried out to investigate electrical stress aging of non-metallic encapsulation materials and limiting material flaws, and to develop a computer model of electrical fields and stresses in encapsulation materials. In addition, a mathematical model was developed and tests were conducted to predict hygroscopic and thermal expansion and contraction on a plastic coated wooden substrate. Thermal cycle and humidity freezing cycle tests, partial discharge tests, and hail impact tests were also carried out. Finally, the effects of soiling on the surface of photovoltaic modules were investigated. Two antisoiling coatings, a fluorinated silane and perflourodecanoic acid were considered.
New gas distributor for fluidized beds prevents hot particles from reacting on it and forming hard crust. In reduction of iron ore in fluidized bed, ore particles do not sinter on distributor and perhaps clog it or otherwise interfere with gas flow. Distributor also relatively cool. In fluidized-bed production of silicon, inflowing silane does not decompose until within bed of hot silicon particles and deposits on them. Plates of spiral distributor arranged to direct incoming gas into spiral flow. Turbulence in flow reduces frequency of contact between fluidized-bed particles and distributor.
An apparatus and method is disclosed for keeping interior walls of a reaction vessel free of undesirable deposits of solid materials in gas-to-solid reactions. The apparatus includes a movable cleaning head which is configured to be substantially complementary to the interior contour of the walls of the reaction vessel. The head ejects a stream of gas with a relatively high velocity into a narrow space between the head and the walls. The head is moved substantially continuously to at least intermittently blow the stream of gas to substantially the entire surface of the walls wherein undesirable solid deposition is likely to occur. The disclosed apparatus and process is particularly useful for keeping the walls of a free-space silane-gas-to-solid-silicon reactor free of undesirable silicon deposits.
Fluidized bed reactor research techniques for fabrication of quartz linears was reviewed. Silane pyrolysis was employed in this fabrication study. Metallic contaminant levels in the silicon particles were below levels detectable by emission spectroscopy.
The growth of silicon on seed particles from the pyrolysis of silane in a fluidized bed reactor (FBR) was studied. The grown particles were shown to be crystalline and to have a structure which has been interpreted to indicate growth by chemical vapor deposition as well as by the collection (scavenging) of silicon clusters on seed particle surfaces. Scanning electron microscopy was used to study the product morphology.
Techniques are being developed to provide lower cost polysilicon material for solar cells. Existing technology which normally provides semiconductor industry polysilicon material is undergoing changes and also being used to provide polysilicon material for solar cells. Economics of new and existing technologies are presented for producing polysilicon. The economics are primarily based on the preliminary process design of a plant producing 1,000 metric tons/year of silicon. The polysilicon processes include: Siemen's process (hydrogen reduction of trichlorosilane); Union Carbide process (silane decomposition); and Hemlock Semiconductor process (hydrogen reduction of dichlorosilane). The economics include cost estimates of capital investment and product cost to produce polysilicon via the technology. Sensitivity analysis results are also presented to disclose the effect of major paramentes such as utilities, labor, raw materials and capital investment.
Silicon deposition on silicon seed particles by silane pyrolysis in a fluidized bed reactor (FBR) was investigated as a low cost, high throughput method to produce high purity polysilicon for solar cell applications. The emphasis of the research is fundamental understanding of fluidized bed silicon deposition. The mechanisms involved were modeled as a six-path process: heterogeneous deposition; homogeneous decomposition; coalescence; coagulation; scavenging; and chemical vapor deposition growth on fines.