By Hydrolyzing Vapor Phase Silicon Compound Patents (Class 423/336)
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Patent number: 6872402Abstract: Pyrogenically prepared silica doped with silver or silver oxide is prepared by feeding an aerosol into a flame such as is used for the preparation of pyrogenic silica, mixing the aerosol homogeneously with gas mixture before the reaction, then allowing the aerosol/gas mixture to react in a flame. The resulting pyrogenic silicas doped with silver or silver oxide are separated from the gas stream. The pyrogenic silica doped with silver or silver oxide by means of an aerosol can be used as a bactericidal filler.Type: GrantFiled: June 19, 2002Date of Patent: March 29, 2005Assignee: Degussa AGInventors: Helmut Mangold, Rainer Golchert
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Patent number: 6835683Abstract: A silica glass member of the present invention is one wherein when a composition thereof is expressed by SiOx, x is not less than 1.85 nor more than 1.95, wherein a concentration of hydrogen molecules included therein is not less than 1×1016 molecules/cm3 nor more than 5×1018 molecules/cm3, and wherein a difference A−B between an absorption coefficient A immediately before an end of irradiation with 1×104 pulses of ArF excimer laser light in an average one-pulse energy density of 2 mJ/cm2 and a second absorption coefficient B at 600 seconds after a stop of the irradiation with the ArF excimer laser light is not more than 0.002 cm−1. When this silica glass member is applied to an illumination optical system and/or a projection optical system in projection exposure apparatus, it becomes feasible to implement uniform exposure while reducing variation in illuminance on a reticle surface and in an exposure area on a wafer.Type: GrantFiled: December 17, 2002Date of Patent: December 28, 2004Assignee: Nikon CorporationInventors: Norio Komine, Akiko Yoshida, Hiroki Jinbo, Seishi Fujiwara
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Patent number: 6800413Abstract: A silylated silica having an SiOH density per nm2 of less than 0.6, based on the BET-method surface area (DIN 66131 and 66132), is prepared by silylating silica in a process where loading, reacting, and purifying are performed in separate steps.Type: GrantFiled: September 9, 2002Date of Patent: October 5, 2004Assignee: Wacker-Chemie GmbHInventors: Herbert Barthel, Mario Heinemann, Franz Grünwald, Helmut Maginot, Ute Völkel
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Publication number: 20040184979Abstract: A method for manufacturing a synthesized silica glass optical member, the method comprising: providing a porous silica glass body; heating the porous' silica glass body in an atmosphere containing hydrogen or oxygen, and sintering the porous silica glass body in an atmosphere containing fluorine compound. Furthermore, a synthesized silica glass optical member manufactured by the method.Type: ApplicationFiled: December 31, 2003Publication date: September 23, 2004Applicant: Shin-Etsu Chemical Co., Ltd.Inventors: Jun Abe, Nobuyasu Mantoku, Shinji Makikawa, Seiki Ejima
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Patent number: 6780393Abstract: A method of producing fine particles of an oxide of a metal, comprising the steps of: preparing an acidic solution which contains ions of the metal; precipitating fine particles of a hydroxide of the metal by adding an alkaline solution to the acidic solution; collecting the fine particles of the hydroxide of the metal precipitated in a mixed solution of the acidic solution and the alkaline solution; mixing fine particles of a carbon with the collected fine particles of the hydroxide of the metal; and heat-treating a mixture of the fine particles of the hydroxide of the metal and the fine particles of the carbon at a predetermined temperature in a non-reducing atmosphere, whereby the fine particles of the oxide of the metal are produced.Type: GrantFiled: December 14, 2001Date of Patent: August 24, 2004Assignees: National Institute of Advanced Industrial Science and Technology, Noritake Co., LimitedInventors: Norimitsu Murayama, Woosuck Shin, Sumihito Sago, Makiko Hayashi
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Patent number: 6763683Abstract: A method and furnace are described for producing a fused oxide body by decomposing a precursor compound of the oxide in a flame to form molten oxide particles and collecting those particles in a furnace constructed of a refractory material to form a fused oxide body, the improvement in the method comprising treating the refractory material with a strong acid in liquid form to react with, and thereby remove, contaminants from at least the surface of the refractory material.Type: GrantFiled: October 23, 2001Date of Patent: July 20, 2004Assignee: Corning IncorporatedInventor: Robert S. Pavlik, Jr.
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Patent number: 6759160Abstract: A silicon oxide powder represented by the formula: SiOx wherein 1.05≦x≦1.5 and having a BET specific surface area of 5-300 m2/g is useful as a negative electrode material to construct a lithium ion secondary cell having a high capacity and improved cycle performance.Type: GrantFiled: February 26, 2002Date of Patent: July 6, 2004Assignee: Shin-Etsu Chemical Co., Ltd.Inventors: Hirofumi Fukuoka, Satoru Miyawaki, Kenji Oõka, Susumu Ueno, Mikio Aramata, Takeshi Fukuda
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Patent number: 6705127Abstract: The present invention is directed to methods of producing soot used in the manufacture of optical waveguides. Both non-aqueous liquid reactants and aqueous solutions containing one or more salts are delivered through an atomizing burner assembly to form a homogenous soot stream containing the oxides of the selected elements contained within the non-aqueous liquid reactant and the aqueous solution. The resulting multi-component soot is collected by conventional methods to form preforms used in the manufacture of optical waveguide fibers. Preforms formed by the methods are also disclosed.Type: GrantFiled: March 12, 2001Date of Patent: March 16, 2004Assignee: Corning IncorporatedInventors: Michael B. Cain, Daniel W. Hawtof, V. Srikant
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Patent number: 6696034Abstract: Hydrophobic silica fine powder is produced by pyrolyzing a silane compound to form a silica fine powder and hydrophobizing the silica fine powder with an organohalosilane as hydrophobizing agent in a fluidization vessel. A portion of the silica fine powder is bypassed to a waste gas line from the fluidization vessel and collected with a cyclone and bag filter, and the collected powder is fed to the fluidization vessel where it is hydrophobized. The amount of unreacted organohalosilane in the waste gases is reduced, alleviating the burden on waste gas treatment. The silica having the unreacted organohalosilane borne thereon is fed back to the fluidization vessel, increasing the reaction efficiency of organohalosilane.Type: GrantFiled: August 30, 2001Date of Patent: February 24, 2004Assignee: Shin-Etsu Chemical Co., Ltd.Inventors: Yasuaki Nozawa, Kiyoshi Shirasuna, Hidekazu Uehara, Keiji Shibata, Susumu Ueno
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Patent number: 6696602Abstract: The present invention relates to a process for the preparation of phosphonomethylglycine, wherein N-phosphonomethyliminodiacetic acid N-oxide is brought into contact with a catalytically effective amount of thiocyanic acid or a salt thereof.Type: GrantFiled: February 6, 2002Date of Patent: February 24, 2004Assignee: BASF AktiengesellschaftInventors: Nicola Christiane Aust, Thomas Butz, Martin Fischer
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Patent number: 6685906Abstract: Silicon oxide containing active silicon represented by the general formula: SiOx wherein x is from 0.8 to 1.9, when analyzed by solid state NMR (29Si DD/MAS) with a sufficient relaxation time set, exhibits a spectrum having two separate peaks, a broad peak (A1) centered at −70 ppm and a broad peak (A2) centered at −110 ppm, the area ratio A1/A2 being in the range of 0.1≦A1/A2≦1.0.Type: GrantFiled: February 2, 2001Date of Patent: February 3, 2004Assignee: Shin-Etsu Chemical Co., Ltd.Inventors: Hirofumi Fukuoka, Mikio Aramata, Kazutoshi Fujioka, Susumu Ueno, Takeshi Fukuda
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Patent number: 6672110Abstract: A method for manufacturing a glass preform includes supplying a first gaseous or vapor phase composition to a reaction chamber; supplying water as a second gaseous or vapor phase composition to the reaction chamber; reacting the water and the first gaseous or vapor phase composition to form an aerosol of glass particles; directing the aerosol along the reaction chamber, out of the reaction chamber, and toward a target; and depositing glass particles of the aerosol onto the target. The first gaseous or vapor phase composition is disposed to provide a hydrolyzable glass precursor. Walls of the reaction chamber have a temperature gradient in which a temperature of the walls increases in a direction of flow of the aerosol along the reaction chamber. Alternatively, a flow of the aerosol along the reaction chamber has a temperature gradient in which a temperature of the aerosol increases in the direction of flow.Type: GrantFiled: December 16, 1999Date of Patent: January 6, 2004Assignee: Pirelli Cavi E Sistemi S.p.A.Inventors: Giacomo Stefano Roba, Marco Arimondi, Donata Piccolo, Sabrina Fogliani
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Patent number: 6649268Abstract: An optical member made of silica glass manufactured by the direct method where a material gas comprising an organosilicon compound is allowed to react in an oxidizing flame, said optical member having a 2×1014 molecules/cm3 or less concentration of formyl radical generated by X-ray irradiation whose dose is 0.01 Mrad or more and 1 Mrad or less.Type: GrantFiled: March 7, 2000Date of Patent: November 18, 2003Assignee: Nikon CorporationInventors: Norio Komine, Seishi Fujiwara, Akiko Yoshida, Hiroki Jinbo, Norihisa Yamaguchi
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Patent number: 6638982Abstract: The invention provides a method of preparing a dispersion of a fumed metal oxide in a liquid carrier comprising the following sequential steps: (a) providing a liquid carrier at a pH that effects dissolution of the metal oxide at a rate the same as or greater than the metal oxide dissolution rate in water at a pH of about 8, (b) mixing with the liquid carrier, in any order, one or more aliquots of both a fumed metal oxide and a metal ion source to form a dispersion, such that the dispersion does not coagulate, and (c) optionally adjusting the pH of the dispersion to the pH of the liquid carrier in step (a). The method allows for the preparation of the dispersion to be done with a high solids loading and at a high pH. Furthermore, the dispersion can have a shelf-life of at least about 1 hour or more at 25° C.Type: GrantFiled: November 14, 2001Date of Patent: October 28, 2003Assignee: Cabot CorporationInventor: Steven E. Brown
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Patent number: 6622523Abstract: The present invention provides a two stage process of thermal separation of CFCs and HCFCs followed by vitrification of the waste into a commercially viable glass. In the first stage, the hydrogenated compounds are reacted at elevated temperature with water and a metal oxide such as calcium oxide to form a halide salt and carbon dioxide. In the second stage of the process, the brine slag is reacted at elevated temperature with the carbon dioxide from stage one and glass-forming raw materials such as silicon dioxide to produce a glass. The final glass product incorporates the halide into the glass.Type: GrantFiled: March 20, 2001Date of Patent: September 23, 2003Inventors: Christopher J. Ludwig, Frederic M. Schwartz
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Patent number: 6590116Abstract: The present invention is directed to a process for purifying siloxane. The invention relates to a method of making a purified siloxane feedstock for use in the manufacturing of silica glass. The invention further relates to solid phase extracting impurities from a polyalkylsiloxane starting material.Type: GrantFiled: October 1, 2001Date of Patent: July 8, 2003Assignee: Corning IncorporatedInventors: Joseph S. Flynn, Dale R. Powers, Brian P. Strines
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Publication number: 20030114572Abstract: There is provided a gel composition having a silica powder and a non-volatile compound. The silica powder particles are spherical and porous. The silica powder has a specific gravity about 0.09 to about 0.6, and is present in an amount about 10 wt % to about 50 wt %. The non-volatile compound is present from about 35 wt % to about 90 wt %. The composition has less than about 5 wt % water. There is also provided a method for imparting a powdery feel to the skin, and a method for treating a cosmetic or medical condition of the skin, nail/cuticle, lips or hair.Type: ApplicationFiled: December 17, 2001Publication date: June 19, 2003Applicant: AVON PRODUCTS, INC.Inventors: Irina Travkina, Lisa Lamberty, Harold Pahlck
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Patent number: 6518210Abstract: A silica glass has a structure determination temperature of 1200 K or lower and an OH group concentration of at least 1,000 ppm. The silica glass is used for photolithography together with light in a wavelength region of 400 nm or shorter.Type: GrantFiled: June 14, 2000Date of Patent: February 11, 2003Assignee: Nikon CorporationInventors: Hiroki Jinbo, Norio Komine, Hiroyuki Hiraiwa
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Patent number: 6455455Abstract: A silicon-aluminum mixed oxide produced by flame hydrolysis and having a composition of from 1 to 99.999 wt. % Al2O3, the remainder being SiO2, which mixed oxide exhibits an amorphous structure in the X-ray diffraction pattern and consists of intergrown primary particles, and in these primary particles crystallites are present. These crystallites having sizes of between one and 200 namometers and the specific surface of the powder being between 5 and 300 m2/g. These products are produced by a process wherein silicon halide and aluminum halide are vaporized in a particular ratio to one another and are homogeneously mixed with air, oxygen and hydrogen in a mixing unit by means of any carrier gas, this mixture undergoes combustion in a burner of known construction and, after the separation of the solids from the vapour phase, any traces of halide possibly adhering to the product are separated off in a further processing step by means of moist air at elevated temperature.Type: GrantFiled: April 28, 2000Date of Patent: September 24, 2002Assignee: Degussa AGInventors: Klaus Deller, Rainer Golchert, Dieter Kerner, Helmut Mangold
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Patent number: 6436524Abstract: When recording using magnetic field modulation recording, the magneto-optical recording medium which is disclosed is capable of satisfactory recording with a low magnetic field. This recording medium is a layered superposition of a recording layer 13 and an auxiliary recording layer 14 having a film thickness of less than or equal to 100 angstroms. The recording layer 13 is a film having an easy perpendicular axis of magnetization whose value of magnetization at room temperature is at least 150 emu/cc, and for example a heavy rare earth—transition metal alloy, a magnetic multilayer film which employs a precious metal, an oxide like a garnet or Spinel ferrite, or some other magnetic alloy may be used. The auxiliary recording layer 14 is typically a heavy rare earth—transition metal alloy, and has a Curie temperature higher (desirably at least 30K higher) than that of the recording layer 13.Type: GrantFiled: January 13, 1998Date of Patent: August 20, 2002Assignee: Seiko Epson CorporationInventors: Masaya Ishida, Takeo Kawase
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Patent number: 6432151Abstract: Disclosed herein is a method of preparing silica slurry for wafer polishing. This method includes pre-treating relatively inexpensive and commercially available fumed or colloidal silica particles as a seed by a settling, a crushing using a ball mill and a paint shaker, and a sonication to produce an aqueous dispersion of the silica particles. The pre-treated silica particles are then combined with tetraethylorothosilicate as a precursor, an alcohol solvent and a base, and grown to a desired size by hydrolysis and polycondensation of the precursor, tetraethylorothosilicate. Then, the alcohol solvent, in which the silica particles are grown, are displaced with water by a vacuum distillation. The resulting aqueous dispersion of the grown silica dispersion is hydrothermally treated in an autoclave. Thus, this method allows the economical preparation of the spherical silica particles having a highly uniform size and a very high purity.Type: GrantFiled: August 22, 2000Date of Patent: August 13, 2002Assignee: Korea Advanced Institute of Science and TechnologyInventors: Jae Hyun So, Min Ho Oh, Sun Hyuck Bae, Seung Man Yang, Do Hyun Kim
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Patent number: 6423331Abstract: Pyrogenically prepared silica doped with silver or silver oxide is prepared by feeding an aerosol into a flame such as is used for the preparation of pyrogenic silica, mixing the aerosol homogeneously with gas mixture before the reaction, then allowing the aerosol/gas mixture to react in a flame. The resulting pyrogenic silicas doped with silver or silver oxide are separated from the gas stream. The pyrogenic silica doped with silver or silver oxide by means of an aerosol can be used as a bactericidal filler.Type: GrantFiled: September 8, 2000Date of Patent: July 23, 2002Assignee: Degussa-Huls AGInventors: Helmut Mangold, Rainer Golchert
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Patent number: 6395807Abstract: The fine spherical silica having a particle size distribution in which maximum particle diameter is 24 &mgr;m, average particle diameter is 1.7 to 7 &mgr;m, and the proportion X1 of particles having a particle diameter of 3 &mgr;m or less in the total particles is 100/D50 to (18+100/D50) wt %, and the viscosity at 50° C. of a mixture obtained by blending a maximum of 80 wt % of the fine spherical silica with a liquid epoxy resin or silicone resin at room temperature is 20 Pa·s or less is provided. The spherical silica is useful as a filler for sealing resin composition which has excellent gap permeability and seals slight gaps, between a substrate and an IC chip and has high reliability.Type: GrantFiled: April 11, 2000Date of Patent: May 28, 2002Assignee: Nippon Chemical Industrial Co., LTDInventors: Yutaka Kinose, Shinsuke Miyabe, Takeshi Sakamoto
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Patent number: 6358486Abstract: Bimodal amporphous inorganic material that in a pore size distribution plot has distinct mesopore and micropore peaks. A process for producing a bimodal material or a material that contains essentially only mesopores involves heating an inorganic oxide in the presence of material that bonds to the inorganic oxide by hydrogen bonding.Type: GrantFiled: September 7, 1999Date of Patent: March 19, 2002Assignee: ABB Lummus Global Inc.Inventors: Zhiping Shan, Thomas Maschmeyer, Jacobus C. (Cornelis) Jansen
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Patent number: 6322765Abstract: The invention relates to a process for preparing highly disperse silicon dioxide by combustion of organochlorosilicon compounds, which comprises transporting a liquid which contains at least one hydrocarbon compound and at least one organochlorosilicon compound into a burner and burning the liquid there in the presence of an oxygen-containing gas and without supply of water.Type: GrantFiled: September 8, 1998Date of Patent: November 27, 2001Assignee: Wacker-Chemie GmbHInventors: Ernst Mühlhofer, Carl-Heinz Ehrke, Gerhard Kalchgruber, Botho Druse
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Patent number: 6217840Abstract: A method for producing fumed silica and a fluorine-containing product from a source of silica in solid form and a solid material containing fluorine, the solid material selected from the group consisting of sodium aluminum tetrafluoride, cryolite, aluminum fluosilicate ammonium bifluoride, sodium aluminum silicofluoride, and sodium fluosilicate. The method comprises the steps of digesting the silica in solid form and the solid material selected from the group consisting of sodium aluminum tetrafluoride, cryolite, aluminum fluosilicate, ammonium bifluoride, sodium aluminum silicofluoride, and sodium flurosilicate in a sulfuric acid digester. The digestion step produces a first gas component comprised of silicon tetrafluoride, hydrogen fluoride and water vapor. The first gas component is removed from the digester.Type: GrantFiled: August 13, 1999Date of Patent: April 17, 2001Assignee: Goldendale Aluminum CompanyInventors: Robert J. Barnett, Michael B. Mezner
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Patent number: 6123908Abstract: A process of treating spent potliner material from aluminum reduction cells and recovering useful products. In the process of the present invention, spent potliner material is introduced into an acid digester containing, for example, sulfuric acid. As a result of this step, a gas component is produced which includes hydrogen fluoride, silicon tetrafluoride and hydrogen cyanide. Also, a slurry component is produced which includes carbon, a refractory material including silica, alumina, sodium compounds such as sodium sulfate, aluminum compounds such as aluminum sulfate, iron compounds such as iron sulfate, magnesium and calcium compounds such as magnesium and calcium sulfate. The slurry component remains in the digester after the gas component is removed. The gas component is recovered and heated an effective amount to convert or decompose the silicon tetrafluoride to fumed silica, hydrogen cyanide to a remaining gas component including CO.sub.2, H.sub.2 O, and nitrogen oxides, as well as HF gas.Type: GrantFiled: March 27, 1999Date of Patent: September 26, 2000Assignee: Goldendale Aluminum CompanyInventors: Robert J. Barnett, Michael B. Mezner
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Patent number: 6071486Abstract: A for producing metal oxide and/or organo-metal oxide compositions from metal oxide and organo-metal oxide precursors utilizing a rate modifying drying agent. The process allows metal oxide and/or organo-metal oxide compositions to be produced from a wide variety of metal oxide and organo-metal oxide precursors including metal halides and organometallic halides.Type: GrantFiled: April 9, 1997Date of Patent: June 6, 2000Assignee: Cabot CorporationInventors: Kenneth C. Koehlert, Douglas M. Smith, William C. Ackerman, Stephen Wallace, David J. Kaul
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Patent number: 6063354Abstract: Pyrogenic oxides having a BET surface area of between 30 and 150 m.sup.2 /g have a viscosity of less than 2,500 mPas in an aqueous suspension. They are prepared by setting the hydrogen ratio gamma and the oxygen ratio lambda to less than one in a high-temperature flame hydrolysis. The pyrogenic oxides are employed in the CMP application in the electronics industry.Type: GrantFiled: January 20, 1998Date of Patent: May 16, 2000Assignee: Degussa AktiengesellschaftInventors: Helmut Mangold, Peer Plambeck-Fischer, Ingo Pauli, Karlheinz Janzon
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Patent number: 6017505Abstract: Preparation of inorganic aerogels based on oxides of the metals magnesium, aluminum, silicon, tin, lanthanum, titanium, zirconium, chromium and/or thorium by producing a hydrogel in a sol/gel process, replacing the water in the hydrogel by an organic solvent, and drying the solvent-moist gel, takes place by conducting the drying step by exposing the solvent-moist gel to an ambient temperature which is above the boiling temperature of the solvent and at a pressure which is below the supercritical pressure of the solvent in such a way that the solvent within the gel is heated up very rapidly and evaporates.Type: GrantFiled: April 14, 1998Date of Patent: January 25, 2000Assignee: BASF AktiengesellschaftInventors: Bernd Ziegler, Thomas Gerber
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Patent number: 5976480Abstract: Pyrogenically produced silica having a specific surface of less than 90 m.sup.2 /g, preferably of less than 60 m.sup.2 /g, and a DBP absorption of less than 60 wt. % (less or equal to 57.30 ml dibutyl phthalate/100 g) is produced by vaporizing silicon halides and/or organosilicon halides, mixing the vapors with a carrier gas, heating the mixture to temperatures definitely above the boiling point of the silicon-halogen compound, mixing with hydrogen and combustion in a known manner in a burner.Type: GrantFiled: July 30, 1996Date of Patent: November 2, 1999Assignee: Degussa-Huls AGInventors: Helmut Mangold, Dieter Kerner, Peter Kleinschmit
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Patent number: 5922299Abstract: This invention pertains to surfactant-templated nanometer-scale porosity of a silica precursor solution and forming a mesoporous material by first forming the silica precursor solution into a preform having a high surface area to volume ratio, then rapid drying or evaporating a solvent from the silica precursor solution. The mesoporous material may be in any geometric form, but is preferably in the form of a film, fiber, powder or combinations thereof. The rapid drying or evaporation of solvent from the solution is accomplished by layer thinning, for example spin casting, liquid drawing, and liquid spraying respectively. Production of a film is by layer thinning, wherein a layer of the silica precursor solution is formed on a surface followed by removal of an amount of the silica precursor solution and leaving a geometrically thinner layer of the silica precursor solution from which the solvent quickly escapes via evaporation.Type: GrantFiled: August 26, 1997Date of Patent: July 13, 1999Assignee: Battelle Memorial InstituteInventors: Paul J. Bruinsma, Suresh Baskaran, Jagannadha R. Bontha, Jun Liu
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Patent number: 5919298Abstract: A method for the preparation of hydrophobic fumed silicas which are useful, for example, as reinforcing fillers in rubber compositions. The method comprises two steps, where in the first step an aqueous suspension of fumed silica is contacted with an organosilicon compound in the presence of a catalytic amount of an acid to effect hydrophobing of the fumed silica. In the preferred method the first step is conducted in the presence of a water miscible organic solvent which facilitates hydrophobing of the fumed silica with the organosilicon compound and the fumed silica has a BET surface area greater than 50 m.sup.2 /g. In the second step the aqueous suspension of the fumed silica is contacted with a water-immiscible organic solvent at a solvent to silica weight ratio greater than 0.1:1 to effect separation of the hydrophobic fumed silica from the aqueous phase. In a preferred process the hydrophobic fumed silica has a surface area within a range of about 100 m.sup.2 /g to 750 m.sup.2 /g.Type: GrantFiled: January 12, 1998Date of Patent: July 6, 1999Assignee: Dow Corning CorporationInventors: Phillip Joseph Griffith, William Herron, Brian Robert Harkness, Rosemary Margaret Taylor, David James Wilson
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Patent number: 5905183Abstract: The instant invention provides a process for reducing chloride content from by-products generated during production of methylchlorosilanes, comprising, (a) hydrolyzing the by-products by combining the by-products with an aqueous medium, the aqueous medium optionally comprising a surfactant, at a pH of at least about 7 and at a temperature above about 0.degree. C. to yield a first phase comprising essentially solids and a second phase comprising an aqueous phase; (b) separating the first and second phase; and (c) oxidizing the solids from the first phase at a temperature of at least about 300.degree. C. for up to about 24 hours to yield a residue comprising less than about 1% by weight of chloride. The solids from the first phase may alternatively be reduced under a hydrogen flow, at a temperature of at least about 500.degree. C. for up to about 24 hours.Type: GrantFiled: June 3, 1997Date of Patent: May 18, 1999Assignee: General Electric CompanyInventors: Michael Lee White, Matthew David Butts, David Cheney DeMoulpied
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Patent number: 5902636Abstract: Dehydroxylated, silica-containing, glass surfaces are known to be at least partially terminated by strained siloxane rings. According to the invention, a surface of this kind is exposed to a selected silane compound or mixture of silane compounds under reaction-promoting conditions. The ensuing reaction results in opening of the strained siloxane rings, and termination of surface atoms by chemical species, such as organic or organosilicon species, having desirable properties. These species can be chosen to provide qualities such as hydrophobicity, or improved coupling to a polymeric coating.Type: GrantFiled: October 17, 1997Date of Patent: May 11, 1999Assignee: Lucent Technologies Inc.Inventors: Alexis Grabbe, Terry Arthur Michalske, William Larry Smith
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Patent number: 5900450Abstract: A method for preparing a three dimensionally connected silica spheres-resin composite, which comprises hydrolyzing and polymerizing a low molecular weight polyalkoxysilane in the presence of an acid catalyst in a mixed solution of the low molecular weight polyalkoxysilane and a water-soluble polymer in a solvent mixture of water and alcohol to obtain a three dimensional connected silica spheres, impregnating the three dimensional connected silica spheres with at least one material selected from resin-forming monomers and resin-forming prepolymers, and curing the material. The composite obtained by the above method retains its strength even at high temperatures where the organic matter undergoes pyrolysis or burnout.Type: GrantFiled: May 22, 1997Date of Patent: May 4, 1999Assignee: Agency of Industrial Science & TechnologyInventors: Yuko Tanaka, Muneaki Yamaguchi, Hiromasa Ogawa, Katsutoshi Tanaka
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Patent number: 5879649Abstract: The present invention is directed to a purified polyalkylsiloxane composition having a boiling point, under atmospheric conditions, of less than about 250.degree. C. and containing high boiling impurities, including siloxanes and silanol-terminated siloxanes, that have boiling points, under atmospheric conditions, of greater than about 250.degree. C. in a total concentration of less than 14 ppm. The present invention is further directed to a method of producing a purified polyalkylsiloxane composition, having a boiling point, under atmospheric conditions, of less than about 250.degree. C., by distilling a polyalkylsiloxane starting material containing high boiling impurities having boiling points, under atmospheric conditions, of greater than about 250.degree. C. in a total concentration of at least 14 ppm, under conditions effective to produce a purified polyalkylsiloxane composition having a boiling point under atmospheric conditions of less than about 250.degree. C.Type: GrantFiled: September 5, 1997Date of Patent: March 9, 1999Assignee: Corning IncorporatedInventors: Danny L. Henderson, Dale R. Powers
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Patent number: 5855860Abstract: Crude fumed silica resulting from pyrogenic hydrolysis is purified by continuously feeding particulate silica and steam or a mixture of steam and air in a steam/air volume ratio of at least 1/2 through an upright column from its bottom toward its top for forming a fluidized bed within the column at a gas linear velocity of 1 to 10 cm/sec. and a temperature of 250.degree. to 400.degree. C., whereby steam deprives the particulate silica of the halide borne thereon, and removing fine particulate silica from which the halide has been eliminated from the top of the column. Using a simple apparatus, pure fine particulate silica is collected at a low cost of energy consumption.Type: GrantFiled: April 29, 1997Date of Patent: January 5, 1999Assignee: Shin-Etsu Chemical Co., Ltd.Inventors: Masanobu Nishimine, Yoshio Tomizawa, Hidekazu Uehara, Kiyoshi Shirasuna, Susumu Ueno
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Patent number: 5776240Abstract: Granules based on silicon dioxide and having the properties:Average particle size: 10 to 120 .mu.mBET surface area: 40 to 400 m.sup.2 /gPore volume: 0.5 to 2.5 ml/gPore size distribution: less than 5% of the total pore volume exists of pores with a diameter<5 nm, remainder are meso- and macroporespH value: 3.6 to 8.5Tapped density: 220 to 700 g/lThey are prepared by dispersing silicon dioxide in water, spray drying, and optionally heating and/or silanizing. The granules can be used as catalyst supports.Type: GrantFiled: February 5, 1996Date of Patent: July 7, 1998Assignee: Degussa AktiengesellschaftInventors: Klaus Deller, Helmfried Krause, Juergen Meyer, Dieter Kerner, Hans Lansink-Rotgerink, Werner Hartmann
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Patent number: 5656250Abstract: A three-dimensional network structure comprising three-dimensionally interconnected spherical silica particles, having specific physical characteristics including diameter, pores on the surfaces of the particles, cross-sectional areas of the bonds interconnecting the spherical silica particles, elasticity modulus, voids content, and silica content, the surfaces of the spherical silica particles being wholly or partly covered with a water-soluble polymer, the network structure being able to remain substantially intact when heat-treated and being able to undergo machining. There is also provided a method of making a three-dimensional network structure comprising spherical silica particles, comprising hydrolyzing and polymerizing a low polymer of an alkoxysilane in a mixed solution containing the alkoxysilane low polymer and a water-soluble polymer in a mixed solvent composed of water and an alcohol in the presence of an acid catalyst.Type: GrantFiled: June 27, 1995Date of Patent: August 12, 1997Assignee: Jiro Hiraishi, Director-General, Agency of Industrial Science and TechnologyInventors: Yuko Tanaka, Muneaki Yamaguchi, Hiromasa Ogawa, Katsutoshi Tanaka
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Patent number: 5580655Abstract: A web-like nanoparticle silica is produced by laser vaporization of silicon metal in a helium/oxygen atmosphere in a diffusion cloud chamber where it aggregates into novel web-like microstructures. The aggregates are porous and have a surface area greater than 300 m.sup.2 /g. Bright blue photoluminescence from the web-like nanoparticle silica is observed upon irradiation with ultraviolet light.Type: GrantFiled: March 3, 1995Date of Patent: December 3, 1996Assignee: Dow Corning CorporationInventors: Mohamed S. S. El-Shall, Daniel Graiver, Udo C. Pernisz
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Patent number: 5395413Abstract: A method of producing a fused silica product comprising introducing a silicon-containing, organometallic compound into a flame to form molten silica particles, and collecting the molten silica particles in a furnace having a crown and cup such that a fused silica product is obtained, wherein at least the furnace crown is formed from a porous, fired, zircon refractory having a sodium ion content of less than 30 ppm. The fused silica product produced by the method has a sodium ion contamination level below 100 parts per billion.Type: GrantFiled: December 16, 1993Date of Patent: March 7, 1995Assignee: Corning IncorporatedInventors: Daniel R. Sempolinski, Latha I. Swaroop
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Patent number: 5342597Abstract: An improved process for uniformly distributing high levels of water in hydrophilic fumed silica by mixing with dry water.Type: GrantFiled: August 6, 1993Date of Patent: August 30, 1994Assignee: Cabot CorporationInventor: Donald E. Tunison, III
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Patent number: 5340560Abstract: A method is provided for making fumed silica aggregate having an average convex perimeter in the range of about 0.12 micron to about 0.6 micron based on the combustion of a mixture of a silicon compound, such as an organosilane, an oxygen containing gas, such as air and a fuel such as hydrogen. The fumed silica aggregate has been found to enhance properties in heat curable filled silicone compositions.Type: GrantFiled: April 30, 1993Date of Patent: August 23, 1994Assignee: General Electric CompanyInventors: Donald F. Rohr, Stanlee T. Buddle, Paul R. Wilson, Michael A. Zumbrum
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Patent number: 5246624Abstract: An aqueous colloidal dispersion of fumed silica, acid and stabilizer, having a fumed silica concentration of at least about 40% by weight. A process for making an aqueous colloidal dispersion is also disclosed.Type: GrantFiled: January 30, 1992Date of Patent: September 21, 1993Assignee: Cabot CorporationInventors: Dennis G. Miller, William F. Moll
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Patent number: 5182095Abstract: A residue from the production of chlorosilanes from raw silicon is treated with steam and aditionally with nitrogen-oxygen mixtures. The resulting residue has a lower chloride content.Type: GrantFiled: July 12, 1991Date of Patent: January 26, 1993Assignee: Huls Troisdorf AktiengesellschaftInventors: Klaus Ruff, Bernhard Falk, Detlef Liesching
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Patent number: 5169809Abstract: The present invention relates to ZrO.sub.2 - and SiO.sub.2 -based ceramic fibers in which the weight ratio between SiO.sub.2 and ZrO.sub.2 is comprised between 99 and 0.7. The tetragonal ZrO.sub.2 phase is stable at temperatures comprised between 0.degree. and 1500.degree. C. The process comprises the preparation of: a solution of Zr(OR.sup.1).sub.4, where R.sup.1 is an alkyl or aryl, Si(OR.sup.2).sub.4, where R.sup.2 is alkyl or aryl, an organic solvent and an acid. Vapor-phase water is bubbled in said solution, then the obtained solution is drawn and the fibers thus obtained are heated to obtain the crystallization of ZrO.sub.2 and SiO.sub.2.Type: GrantFiled: January 25, 1990Date of Patent: December 8, 1992Assignee: SNIA Fibre S.p.A.Inventors: Umberto Brenna, Giovanni Carturan, Gianmarco Del Felice, Mirto Mozzon
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Patent number: 5158758Abstract: A method for production of high specific surface area silica gel by hydrolysis of silicon tetrahalide, wherein a solution of silicon tetrahalide in a non-reactive solvent such as alcohol is mixed with water to produce silica gel having a high surface area and narrow pore diameter distribution especially suited for use as normal phase packing material in high performance chromatography columns. The water contains fluoride ions if the halide is chloride. Reverse phase packing material can be prepared by reacting the normal phase silica gel with organochlorosilanes to prepare bonded reverse phase material for use in high performance liquid chromotagraphy systems.Type: GrantFiled: April 24, 1989Date of Patent: October 27, 1992Assignee: International Minerals & Chemical Corp.Inventors: Paul C. Chieng, Deborah J. Brame, Alexander H. T. Chu
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Patent number: 5152819Abstract: This invention relates to the production of high purity fused silica glass through oxidation and/or flame hydrolysis of a halide-free, organosilicon-R compound in vapor form having the following properties:(a) producing a gas stream of a halide-free silicon-containing compound in vapor form capable of being converted through thermal decomposition with oxidation or flame hydrolysis to SiO.sub.2 ;(b) passing said gas stream into the flame of a combustion burner to form amorphous particles of fused SiO.sub.2 ;(c) depositing said amorphous particles onto a support; and(d) either essentially simultaneously with said deposition or subsequently thereto consolidating said deposit of amorphous particles into a virtually nonporous body; the improvement comprising utilizing a halide-free, organosilicon-R compound in vapor form having the following properties:(1) a Si--R bond dissociation energy that is no higher than the dissociation energy of the Si--O bond;(2) a boiling point no higher than 350.degree. C.Type: GrantFiled: August 26, 1991Date of Patent: October 6, 1992Assignee: Corning IncorporatedInventors: Jeffery L. Blackwell, Michael S. Dobbins, Robert E. McLay, Carlton M. Truesdale
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Patent number: 5043002Abstract: This invention relates to the production of high purity fused silica glass through oxidation or flame hydrolysis of a vaporizable silicon-containing compound. More particularly, this invention is directed to the use of vaporizable, halide-free compounds in said production. In the preferred practice, a polymethylsiloxane comprises said vaporizable, halide-free compound.Type: GrantFiled: August 16, 1990Date of Patent: August 27, 1991Assignee: Corning IncorporatedInventors: Michael S. Dobbins, Robert E. McLay