Abstract: A process for producing silane by reacting a silicon halide with highly reactive magnesium and a cyclic process for producing silane by reacting magnesium hydride with a silicon halide, reacting the magnesium halide as formed with an alkali metal to recover elemental magnesium, and pressure hydrogenating said magnesium to form magnesium hydride and repeat the cycle. A highly reactive magnesium hydride is formed by the homogeneously catalyzed pressure hydrogenation of magnesium, preferably using an activated transition metal catalyst such as TiCl.sub.4 and a polycyclic organic compound such as anthracene. The highly activated magnesium hydride is thereafter used for reaction with silicon halide to produce silane.

Abstract: A process for producing silane, which comprises forming a powdery mixture by mixing silica powder recovered from geothermal hot water with metallic magnesium powder, heating and reducing said powdery mixture to convert it to magnesium silicide and then reacting an organic acid with said magnesium silicide to produce silane and recovering said silane.

Abstract: Silicon hydrides are produced by acid hydrolysis of ternary silicon alloys. According to the process there are made to react an industrial ternary alloy of the formula M.sub.x M.sup.2.sub.y Si.sub.z, in which M.sup.1 is a reducing metal, M.sup.2 is an alkali alkaline-earth metal, with a dilute acid selected from hydracids and orthophosphoric acid, at a concentration of 2N to 6N, by adding the ternary alloy in the form of fine powder to the acid, the reaction being preformed between ambient temperature and 90.degree. C. The various hydrides are condensed, and separated by fractional evaporation under partial vacuum. The silicon hydrides--silane, disilane and higher polysilanes--after purification can be used as silicon vectors, depending on their chemical nature, particularly in the industries of electronic components, photovolaitic cells, photocopier drums and for frosting light bulbs by the dry method.

Abstract: Disclosed is a method for making silane. A silicon tetrahalide having the general formula SiX.sub.4 is reacted with a compound which can be alcohols to C.sub.4, alkanes to C.sub.4, alkenes to C.sub.4 alkenes to C.sub.4 or a mixture thereof, where X is independently selected from the halogens, to produce a product having the general formula SiR.sub.4, where each R is independently selected from alkoxy to C.sub.4, alkyl to C.sub.4, alkylene to C.sub.4 and alkenyl to C.sub.4. The SiR.sub.4 is then reacted with hydrogen to produce the silane.

Abstract: Silicon tetrachloride, hydrogen and metallurgical silicon are reacted at about 400.degree.-600.degree. C. and at pressures in excess of 100 psi, and specifically from about 300 up to about 600 psi to form di- and trichlorosilane that is subjected to disproportionation in the presence of an anion exchange resin to form high purity silane. By-product and unreacted materials are recycled, with metallurgical silicon and hydrogen being essentially the only consumed feed materials. The silane product may be further purified, as by means of activated carbon or cryogenic distillation, and decomposed in a fluid bed or free space reactor to form high purity polycrystalline silicon and by-product hydrogen which can be recycled for further use. The process results in simplified waste disposal operations and enhances the overall conversion of metallurgical grade silicon to silane and high purity silicon for solar cell and semiconductor silicon applications.

Abstract: A method of forming preceramic polymers by mixing (A) a methylpolysilane of the formula [(RSiH).sub.x (RSi).sub.y ].sub.n, (where R is a lower alkyl group having from 1 to about 6 carbon atoms, a cycloalkyl group having from 3 about to 6 carbon atoms, a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, a tri(lower)alkyl- or di(lower)alkylsilyl group x+y=1, (x and y are each >0 and also x=l, y=o), and n is an integer greater than 1 with (B) an organic or organisilicon compound having at least two alkenyl groups and allowing the mixture to react is disclosed. Preferably, the alkenyl group is a vinyl group. The reaction is preferably initiated by the generation of reactive free radicals. Novel preceramic polymers formed by this method are also disclosed.

Abstract: Disilane Si.sub.2 H.sub.6 is obtained with good yield by reduction reaction of Si.sub.2 Cl.sub.6 with a mixture of LiH and LiAlH.sub.4 in an organic liquid medium such as n-butyl ether. Usually the reaction temperature is -25.degree. C. to 50.degree. C. A suitable range of the mole ratio of LiH to LiAlH.sub.4 is from 0.8 to 40. It is impracticable to reduce Si.sub.2 Cl.sub.6 to Si.sub.2 H.sub.6 by using LiH alone as the reducing agent, but the reaction proceeds smoothly when a LiH/LiAlH.sub.4 mixture is used. The use of the mixture is economically advantageous over the use of expensive LiAlH.sub.4 alone.

Abstract: A process for the production of high purity silane by reacting silicon tetrafluoride exclusively with sodium aluminum tetrahydride, potassium aluminum tetrahydride, or a mixture of sodium aluminum tetrahydride and potassium aluminum tetrahydride, preferably in an inert liquid reaction medium comprising an ether. The inventive process is a highly advantageous and economical route to silane since it also produces valuable fluoride salt.

Abstract: A process for producing silane, whereby silicon tetrafluoride is reacted with magnesium hydride in a melt of alkali or alkaline earth halides under a hydrogen partial pressure which is greater than the dissociation pressure of the magnesium hydride at the temperature of the melt.

Abstract: The process of disproportionation of chlorosilanes in the presence of a dried catalyst which is dried by heating up to 200.degree. C. under vacuum starting from a water-containing anion exchange cross-linked resin matrix containing as a functional group and said resin matrix stable at temperatures up to about 200.degree. C. without separation of the functional group from the resin matrix to produce the disproportionated product of high purity, semiconductor grade, without any contamination from the catalyst.

Abstract: There is disclosed a redistribution catalyst which is the reaction product of a quaternary ammonium halide salt or tertiary amine, and an inorganic carrier having surface hydroxyl groups, such as silica, zeolite, clays, and silicone resins. The catalyst is useful for the disproportionation of chlorosilicon hydrides to dichlorosilane and silane at reaction conditions including a temperature from 0.degree. to 200.degree. C., in liquid or vapor phase with a pressure from 0.1 to 10 atmospheres.

Abstract: A process for producing silicon hydrides represented by the general formula Si.sub.n H.sub.2n+2 wherein n is a positive integer of 1 to 6, which comprises reacting a silicon-containing alloy with an aqueous solution of an acid in the presence of at least one inert organic solvent having a boiling range of from -60.degree. C. to 250.degree. C.

Abstract: A chlorosilane disproportionation catalyst comprising a tertiary amine of the formula: ##STR1## where each R represents an aliphatic hydrocarbon group and the sum of carbon atoms in the three aliphatic hydrocarbon groups as R is 12 or more, and a tertiary amine hydrochloride of the formula: ##STR2## where R is as defined above.

Abstract: Silane, well adopted as a source of semiconductor/photovoltaic grade silicon, is facilely prepared from methyldichlorosilane and trichlorosilane and/or tetrachlorosilane by, (A) in a first step catalytically redistributing methyldichlorosilane with trichlorosilane or tetrachlorosilane, or admixture thereof, to form methyltrichlorosilane and dichlorosilane, and separating dichlorosilane from the resulting reaction medium, and (B) in a second step, catalytically disproportionating the dichlorosilane thus separated to form silane and trichlorosilane, and thence recovering silane thus formed and optionally recycling trichlorosilane to said step (A).

Abstract: Silane is efficiently converted to disilane by irradiation at pressures in excess of about 75 torr using pulsed coherent light having a wavelength in the range from about 10.2 to about 11.2 .mu.m.

Abstract: A purifier for purifying a raw material gas for use in manufacturing semiconductor devices is formed by a hydrogenated amorphous substance of an element selected from a group consisting of Si, Ge, P and As whose hydride gas is used as the raw material gas. This purifier is used for purifying the raw material gas to be purified in such a manner that the raw material gas is brought into contact with the purifier comprising the hydrogenated amorphous substance which is maintained at a temperature a little lower than the decomposition temperature of the raw material gas to efficiently remove the small amount of oxygen from the raw material gas.

Abstract: Silane, SiH.sub.4, and diochlorosilane, particularly suitable for the preparation of silicon are readily obtained by disproportionating trichlorosilane to dichlorosilane and, ultimately silane by reacting:(a) a silane containing at least one Si-H bond, of the general formula R.sub.n H.sub.m SiX.sub.4-(n+m) wherein R represents an alkyl or aryl group, x represents a halogen or an alkoxy group, n is an integer equal to 0, 1, 2 or 3 and m is an integer equal to 1, 2 or 3, and(b) a catalyst system comprising an ionic inorganic salt of the formula M.sup.+ A.sup.- and a compound capable of at least partially dissociating the salt by complexing its cation M.sup.+.

Abstract: In preparing of silicon hydrides with use of a mixture of an alkyl aluminum hydride and a trialkyl aluminum as a reducing agent for a silicon compound, an aluminum halide compound is added to said mixture in an amount sufficient for converting at least 90 mol % of the trialkyl aluminum to a dialkyl aluminum monohalide prior to the reduction reaction. Silicon hydrides are obtained with a high yield and quality.

Abstract: An improved process is disclosed for the high pressure plasma hydrogenation of silicon tetrachloride. Hydrogen and silicon tetrachloride are reacted in the presence of a high pressure plasma and further in the presence of a boron catalyst to form trichlorosilane and dichlorosilane. By adding the boron catalyst the overall conversion efficiency is increased and the dichlorosilane content in the reaction effluent is increased.

Abstract: Elemental silicon is produced by a process and apparatus wherein relatively impure silane (SiH.sub.4) is purified in the gaseous state, while mixed with an inert carrier gas, to a content of electronically active impurities which is no higher than that of "electronic grade" silicon. The silane so purified is then thermally decomposed to form elemental silicon of electronic grade purity, without need for further purification of the elemental silicon itself. The silane purification is carried out by injecting the impure silane gas as a series of timed, spaced pulses into a carrier gas stream which transports the silane pulses to a gas chromatographic column, through which the pulses flow in sequence. The column has a porous polymer or a molecular sieve packing which is specially preconditioned to achieve high resolution separation of the components of the feed.

Abstract: A process for the removal of and analysis of phosphine and arsine impurities in silane gas. Silane gas which normally contains the impurities of AsH.sub.3 and PH.sub.3 is contacted with a solution of NaAlH.sub.4 in dimethoxyethane, other ether or amine to remove the impurities therefrom. The dimethoxyethane or other ether solution may then be hydrolyzed with water or alcohol to evolve hydrogen gas from the NaAlH.sub.4 and to re-evolve phosphine and arsine which may then be quantitatively determined by gas chromatography, atomic absorption, or other means.

Abstract: A battery of special burners, each adapted for the treatment of a particular range of waste material formed during the conversion of metallurgical grade silicon to high purity silane and silicon, is accompanied by a series arrangement of filters to recover fumed silica by-product and a scrubber to recover muriatic acid as another by-product. All of the wastes are processed, during normal and plant upset waste load conditions, to produce useful by-products in an environmentally acceptable manner rather than waste materials having associated handling and disposal problems.

Abstract: Essentially pure silane, SiH.sub.

Abstract: What is disclosed is a process for preparing R.sub.3 'SiNH-containing metallosilazane polymer containing boron, titanium, or phosphorous by contacting and reacting chlorine-containing disilanes and certain reactive metal halides with [R.sub.3 'Si].sub.2 NH where R' is vinyl, hydrogen, or alkyl radical of 1-3 carbon atoms, or phenyl. Preferred reactive metal halides include BBr.sub.3, TiCl.sub.4, and PCl.sub.3. The metallosilazane polymers are useful as chemical intermediates to provide silicon-containing chemical compounds. The metallosilazane polymers are also useful in the formation of ceramic material. The ceramic materials may be formed by heating the metallosilazane polymer at elevated temperatures in an inert atmosphere or in a vacuum.

Abstract: A process for the coproduction of silane and AlF.sub.3 is described. SiF.sub.4 and amine alane (AlH.sub.3.NR.sub.3) complexes are reacted to produce gaseous silane and AlF.sub.3 coproduct. The amine tends to complex somewhat with coproduct AlF.sub.3 but is released therefrom by heating. AlF.sub.3 is a very saleable commodity thereby making the invention an improvement over other hydride reactions which produce less usable coproducts.

Abstract: A hydrogen-containing silicic substance comprising a four-coordinate Si lattice surrounded by a shell of SiH.sub.2 and/or SiH.sub.3 is disclosed. The substance contains unbound hydrogen in the Si lattice, making it possible to conveniently store hydrogen.

Abstract: A storage material for hydrogen comprised of amorphous silicon containing phosphorous, in addition to hydrogen (a-Si:H:P). In certain embodiments, such storage material is produced via a glow discharge plasma from a reactive gas mixture in accordance with a fluidized bed method or by quenching a phosphorous-doped silicon melt at a relatively high cooling rate. By admixing phosphorous with silicon, the absorption capacity of the resultant phosphorous-doped silicon material for hydrogen can be increased by a factor of 2 with the same production temperatures (200.degree. C.). The storage material is useful in energy storage tanks (cheap and easily mass-produced).

Abstract: Silicon tetrafluoride is reacted with sodium hydride in a cyclic ether reaction medium such as tetrahydrofuran or 1,4-dioxane or in dimethoxyethane. Sodium aluminum hydride is dissolved in the solvent and catalyzes the reaction in amounts of 4-25%, by weight of combined sodium hydride and sodium aluminum hydride.

Abstract: The dismutation/redistribution of halogenosilanes into silane is carried out by contacting at least one halogenosilane comprising at least one Si-H function with a compound comprising at least one .alpha.-oxoamine group, then by contacting the products of such reaction with a compound also comprising at least one .alpha.-oxoamine group, to selectively dissolve all products of reaction except for the silane therein, and then separating the desired silane therefrom.

Abstract: Silane, a useful intermediate in the production of silicon, is facilely quantitatively prepared by hydrogenating chlorosilanes in a bath of molten salts, said molten bath comprising a ternary mixture of lithium chloride and two other metal chlorides, such two other metal chlorides being either two different alkaline earth metal chlorides, or one alkaline earth metal chloride and one alkali metal chloride, or two different alkali metal chlorides, and said ternary mixture having a melting point not in excess of about 400.degree. C.

Abstract: Polyvinyl cyclic tertiary amine hydrocarbons having nitrogen in the ring as catalysts for chlorosilane disproportionation. The catalysts are suitable for continuous flow processes redistributing any one or more of SiHCl.sub.3, SiH.sub.2 Cl.sub.2, and SiH.sub.3 Cl.

Abstract: A silicon halide such as silicon tetrafluoride is reacted with an agitated slurry of an alkali metal hydride such as sodium hydride in a liquid which includes a diaryl ether such as diphenyl ether. At elevated temperatures such as 250.degree.-260.degree. C., complete conversion of the silicon tetrahalide to silane is observed, even with contact times under two seconds.

Abstract: Silica having an enhanced level of dehydration beyond what can be produced by heating alone is produced by a three step process comprising (1) chlorination, (2) dechlorination, and (c) oxidation. The resulting dehydroxylated silica is a novel composition of matter and is useful as a reinforcing agent in rubber or plastics and as a support for a chromatographic column in addition to being suitable for a catalyst support. Where the dechlorinating agent is hydrogen, a hydrophobic silica composition containing.tbd.Si-H structures and essentially no -OH groups is produced which is suitable for use as a reducing agent, a coupling agent as well as a precursor for the oxidized dehydroxylated silica described above. The resulting composition is particularly suitable as a support for chromium-containing olefin polymerization catalysts.

Abstract: A process for controlling the dihydride and monohydride bond densities in hydrogenated amorphous silicon produced by reactive rf sputtering of an amorphous silicon target. There is provided a chamber with an amorphous silicon target and a substrate therein with the substrate and the target positioned such that when rf power is applied to the target the substrate is in contact with the sputtering plasma produced thereby. Hydrogen and argon are fed to the chamber and the pressure is reduced in the chamber to a value sufficient to maintain a sputtering plasma therein, and then rf power is applied to the silicon target to provide a power density in the range of from about 7 watts per square inch to about 22 watts per square inch to sputter an amorphous silicon hydride onto the substrate, the dihydride bond density decreasing with an increase in the rf power density. Substantially pure monohydride films may be produced.

Abstract: Tri- and dichlorosilanes formed by hydrogenation in the course of the reaction of metallurgical silicon, hydrogen and recycle silicon tetrachloride are employed as feed into a separation column arrangement of sequential separation columns and redistribution reactors which processes the feed into ultrahigh purity silane and recycle silicon tetrachloride. A slip stream is removed from the bottom of two sequential columns and added to the recycle silicon tetrachloride process stream causing impurities in the slip streams to be subjected to reactions in the hydrogenation step whereby waste materials can be formed and readily separated.

Abstract: Silica having an enhanced level of dehydration beyond what can be produced by heating alone is produced by a three step process comprising (1) chlorination, (2) dechlorination, and (c) oxidation. The resulting dehydroxylated silica is a novel composition of matter and is useful as a reinforcing agent in rubber or plastics and as a support for a chromatographic column in addition to being suitable for a catalyst support. Where the dechlorinating agent is hydrogen, a hydrophobic silica composition containing .tbd.Si--H structures and essentially no --OH groups is produced which is suitable for use as a reducing agent, a coupling agent as well as a precursor for the oxidized dehydroxylated silica described above.

Abstract: Process for the disproportionation of a chlorosilicon hydride which comprises contacting it with an ion exchange resin containing tertiary amino or quaternary ammonium group bonded therein. There is described a cyclic process in which a fixed bed of the resin may be employed.

Abstract: A process for the purification of a mixture of silane and impurities comprising passing the mixture through a succession of zones connected in series, in a closed system, according to the following steps:(a) passing the mixture, in gaseous form, through a zone containing porous, granular charcoal as an adsorbent at a temperature in the range of about minus 40.degree. C to about minus 80.degree. C to provide a mixture of silane and remaining impurities in gaseous form;(b) passing the gaseous mixture from step (a) through a zone containing porous, granular magnesium silicate as a adsorbent at a temperature in the range of about minus 40.degree. C to about minus 80.degree. C to provide a mixture of silane and remaining impurities in gaseous form;(c) passing the gaseous mixture from step (b) into a distillation zone in such a manner that the impurities are removed overhead in gaseous form and at least about 95 per cent by weight of the silane is converted to liquid bottoms; and(d) recovering the bottoms.

Abstract: The present invention relates to a process for preparing high yields of hydrosilanes by reacting methylchloropolysilanes with hydrogen gas under pressure at a temperature of from about 25.degree. C to about 350.degree. C in the presence of a copper catalyst. Useful copper catalysts include copper metal, copper salts, and complexes of copper salts with organic ligands.

Abstract: A process for the production of silane in a reaction vessel comprising (i) a single closed chamber, (ii) a hollow tube open at both ends, said tube being disposed in the lower portion of the chamber; and (iii) means for circulating liquid in the lower portion of the chamber in such a manner that the liquid flows in a downward direction through the tube and in an upward direction outside of the tubeComprising the following steps:A. maintaining a melt of lithium chloride in the lower portion of the chamber, the level of the melt being above the tube;B. activating the circulating means;C. introducing liquid lithium into the melt in such a manner that at least a part thereof is brought to the surface of the melt;D. introducing hydrogen gas above the surface of the melt in such a manner that hydrogen gas reacts with lithium at the surface of the melt to form lithium hydride,The lithium, lithium hydride, and melt being admixed by the circulating means to provide a homogeneous mixture thereof;E.

Abstract: A process for preparing monosilane and low silane esters thereof which comprises contacting a hydrogen silane ester of the formula H.sub.x Si(OR).sub.4.sub.-x, wherein R represents an alkyl or alkoxyalkyl moiety and x is 1, 2 or 3, with a catalyst of an element of the first group and/or the second or third main or secondary group of the periodic system or iron or manganese or and organic nitrogen compound under distillation conditions and recovering a product having the formula H.sub.x.sub.+1 Si(OR).sub.4.sub.-x.sub.-1 and/or a product of the formula H.sub.x.sub.-1 Si(OR).sub.4.sub.-x.sub.+1.

Abstract: There is a process for manufacturing SiH.sub.4 by the disproportionation or redistribution of HSiCl.sub.3 which comprises feeding HSiCl.sub.3 into a bed of insoluble solid anion exchange resin containing tertiary amino or quaternary ammonium groups bonded to carbon therein, refluxing the HSiCl.sub.3 to vaporize disproportionated products to the upper portion of the bed and condensing liquid SiCl.sub.4 from the area in which HSiCl.sub.3 is refluxed, maintaining the temperature at the top of the bed above the boiling point of SiH.sub.4 and below the boiling point of H.sub.3 SiCl, and recovering SiH.sub.4 from the bed substantially free of chlorosilanes.