US3508954A - Silicon carbide structures - Google Patents

Silicon carbide structures Download PDF

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Publication number
US3508954A
US3508954A US3508954DA US3508954A US 3508954 A US3508954 A US 3508954A US 3508954D A US3508954D A US 3508954DA US 3508954 A US3508954 A US 3508954A
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Prior art keywords
chamber
silicon
carbide
filament
deposition
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Expired - Lifetime
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Rudolph C White
Harold R Davis
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Texaco Inc
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Texaco Inc
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/90Carbides
    • C01B32/914Carbides of single elements
    • C01B32/956Silicon carbide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/10Particle morphology extending in one dimension, e.g. needle-like
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913Rod, strand, filament or fiber
    • Y10T428/2933Coated or with bond, impregnation or core
    • Y10T428/294Coated or with bond, impregnation or core including metal or compound thereof [excluding glass, ceramic and asbestos]
    • Y10T428/296Rubber, cellulosic or silicic material in coating
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913Rod, strand, filament or fiber
    • Y10T428/2933Coated or with bond, impregnation or core
    • Y10T428/2962Silane, silicone or siloxane in coating
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913Rod, strand, filament or fiber
    • Y10T428/298Physical dimension

Description

A ril 28, 1970 R. c. WHITE ETAL SILICON CARBIDE STRUCTURES Filed 5, 1967 co m 0 v cu I u o INVENTORS RUDOLPH C. WHITE '7 HAROLD R. DAWS ATTORNEYfi United States Patent 3,508,954 SILICON CARBIDE STRUCTURES Rudolph C. White, Midlothian, and Harold R. Davis,

Richmond, Va., assignors, by mesne assignments, to Texaco Inc., New York, N.Y., a corporation of Delaware Filed Oct. 5, 1967, Ser. No. 673,054

Int. Cl. C23c 11/00 US. Cl. 117106 3 Claims ABSTRACT OF THE DISCLOSURE Silicon carbide structures are made by heating a refractory substrate to a temperature of from about 2100" F. to about 2500 F. in an atmosphere of methyltrichlorosilane, methyldichlorosilane and hydrogen. The method is particularly useful for the production of filaments of high tensile strength and high elastic modulus.

The invention relates to a method of producing silicon carbide filaments and other structures combining a high tensile strength and high elastic modulus with hardness and resistance to oxidation.

We have found that structures having useful combinations of the desired physical and chemical properties can be produced by depositing a layer of silicon carbide on a refractory substrate by heating the substrate to a temperature of from about 2100 to about 2500 F. in an atmosphere containing methyldichlorosilane and methyltrichlorosilane in the proportion of from about 1 to 3 to about 1 to by volume and from about 50% to about 80% by volume of hydrogen.

The method of the invention is particularly suitable for the production at high rates of deposition of oxidation resistant filaments having high tensile strength of the order of 400x10 p.s.i. and modulus values upwards of 60x10 p.s.i. which are useful in the production of composite structural members having various applications such as high strength lightweight airfoils, by incorporating the filaments in a plastic, elastic, vitreous, cementitious or metallic matrix Particularly useful as substrates for the silicon carbide structures are filaments of conductive refractory substances such as tungsten, rhenium, tantalum, titanium, molybdenum, iron, copper, nickel and nichrome.

An illustrative example of the method of the invention will be described with reference to the accompanying drawing which is a diagrammatic representation of apparatus useful in practising the invention.

The apparatus shown in the drawing comprises a preheating chamber generally designated 10 and a silicon carbide deposition chamber generally designated 11. A substrate filament 12 is passed continuously at a substantially uniform rate of travel from power-driven feed spool 13 successively through the preheating chamber and the silicon carbide deposition chamber to power-driven takeup spool 14. The preheating chamber and the deposition chamber are sealed from each other and from the surrounding atmosphere by means of Y-shaped mercury seals 15 connected by flexible tubes 24 to separate level adjusting reservoirs 16. The mercury seals also serve as contactors for the supply of heating current to the substrate filament in the preheating and deposition chambers. Tension on the substrate filament is maintained substantially constant by suspending a tensioning weight 26 in a loop of the filament. Ts 17 and associated T-connectors 18 serve as inlets and outlets for gases into and out of the preheating and deposition chambers and also for the support of adjustable guide loops 19 for the substrate filament.

3,508,954 Patented Apr. 28, 1970 Hydrogen or other purging gas may be supplied to preheating chamber 10 through tube 20 and removed through tube 21 for the purpose of removing absorbed, adsorbed or reacted oxygen from the surface of the substrate filament as it passes through chamber 10. Lubricants or other surface impurities are also removed from the filament by evaporation or by reaction with the hydrogen.

Heat-jacketed vessels 25 provide means for vaporizing the methylhalogensilanes and causing the vapor to flow through suitable metering devices 28 into a mixing chamber 29 into which hydrogen may be introduced through pipe 30. The mixture of hydrogen and methylhalogensilanes is supplied to chamber 11 through tube 22 and residual gases and vapors pass out of chamber 11 through tube 23 to recovery or disposal means (not shown).

Glass is a suitable material of construction for the preheating and deposition chambers and for the connections thereto and therebetween. The flexible tubing can be made of polyethylene and the T-connectors 18 can be of copper.

Instead of introducing the methylhalogensilane and hydrogen mixture into one end of chamber 11, the mixture may be introduced at the middle of the chamber and the residual gases and vapor removed at the two ends or the mixture may be introduced at the two ends and the residual gases and vapors removed at the middle of the chamber. Also, instead of using a single silicon carbide deposition chamber, the deposition may be carried out in a plurality of serially connected chambers under the same or different operating conditions.

The following is a representative example of the operation of the method of the invention:

A 0.5 mil tungsten wire is passed through the apparatus at a speed of about 5 feet per minute. It is heated to about 2200 F. in a current of hydrogen in the preheating chamber 10. In the five foot silicon carbide deposition chamber 11 it is heated to about 2300" F. A mixture of 30% by volume of methyltrichlorosilane and 5% by volume of methyldichlorosilane in hydrogen is supplied to the chamber resulting in the deposition of silicon carbide to an overall filament diameter of about 4 mils.

We claim:

1. A method of making silicon carbide structures which comprises heating a refractory substrate to a temperature of from about 2100 to about 2500 F. in an atmosphere containing methyldichlorosilane and methyltrichlorosilane in the proportion of from about 1 to} to about 1 to 10 by volume and from about 50% to about by volume of hydrogen.

2. A method of making silicon carbide filaments which comprises passing a refractory filament through an atmosphere containing methyldichlorosilane and methyltrichlorosilane in the proportion of from about 1 to 3 to about 1 to 10 by volume and from about 50% to about 80% by volume of hydrogen while heating the refractory filament to a temperature from about 2100 to about 2500 F.

3. A method as defined in claim 2 wherein the refractory filament is tungsten.

References Cited UNITED STATES PATENTS 3,157,541 11/1964 Heywang et al.

FOREIGN PATENTS 145,106 1962 U.S.S.R.

ANDREW G. GOLIAN, Primary Examiner US. Cl. X.R. 23208

US3508954A 1967-10-05 1967-10-05 Silicon carbide structures Expired - Lifetime US3508954A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3643658A (en) * 1968-09-03 1972-02-22 Straumann Inst Ag Implants of titanium or a titanium alloy for the surgical treatment of bones
US4295890A (en) * 1975-12-03 1981-10-20 Ppg Industries, Inc. Submicron beta silicon carbide powder and sintered articles of high density prepared therefrom
US5609912A (en) * 1995-09-08 1997-03-11 Georgia Tech Research Corp. Ceramic fabric forming method
US20030204259A1 (en) * 2000-12-13 2003-10-30 Goble E. Marlowe Multiple facet joint replacement
US20050131409A1 (en) * 2003-12-10 2005-06-16 Alan Chervitz Linked bilateral spinal facet implants and methods of use
US20050234551A1 (en) * 2001-03-02 2005-10-20 Facet Solutions, Inc. Method and apparatus for spine joint replacement
US7041136B2 (en) 2000-11-29 2006-05-09 Facet Solutions, Inc. Facet joint replacement
US20060200149A1 (en) * 2005-02-22 2006-09-07 Hoy Robert W Polyaxial orhtopedic fastening apparatus
US20060217718A1 (en) * 2005-03-28 2006-09-28 Facet Solutions, Inc. Facet joint implant crosslinking apparatus and method
US20080167688A1 (en) * 2005-02-22 2008-07-10 Facet Solutions, Inc. Taper-Locking Fixation System
US20080221622A1 (en) * 2007-01-10 2008-09-11 Facet Solutions, Inc. Facet Joint Replacement
US7507242B2 (en) 2004-06-02 2009-03-24 Facet Solutions Surgical measurement and resection framework
US7566345B1 (en) 2001-03-01 2009-07-28 Facet Solutions, Inc Prosthesis for the replacement of a posterior element of a vertebra
US7722647B1 (en) 2005-03-14 2010-05-25 Facet Solutions, Inc. Apparatus and method for posterior vertebral stabilization
US8556936B2 (en) 2000-11-29 2013-10-15 Gmedelaware 2 Llc Facet joint replacement
US8562649B2 (en) 2004-02-17 2013-10-22 Gmedelaware 2 Llc System and method for multiple level facet joint arthroplasty and fusion

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3157541A (en) * 1958-10-23 1964-11-17 Siemens Ag Precipitating highly pure compact silicon carbide upon carriers

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3157541A (en) * 1958-10-23 1964-11-17 Siemens Ag Precipitating highly pure compact silicon carbide upon carriers

Cited By (53)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3643658A (en) * 1968-09-03 1972-02-22 Straumann Inst Ag Implants of titanium or a titanium alloy for the surgical treatment of bones
US4295890A (en) * 1975-12-03 1981-10-20 Ppg Industries, Inc. Submicron beta silicon carbide powder and sintered articles of high density prepared therefrom
US5609912A (en) * 1995-09-08 1997-03-11 Georgia Tech Research Corp. Ceramic fabric forming method
US7621955B2 (en) 2000-11-29 2009-11-24 Facet Solutions, Inc. Facet joint replacement
US8313511B2 (en) 2000-11-29 2012-11-20 Gmedelaware 2 Llc Facet joint replacement
US8556936B2 (en) 2000-11-29 2013-10-15 Gmedelaware 2 Llc Facet joint replacement
US7618453B2 (en) 2000-11-29 2009-11-17 Facet Solutions, Inc Facet joint replacement
US7041136B2 (en) 2000-11-29 2006-05-09 Facet Solutions, Inc. Facet joint replacement
US20070185576A1 (en) * 2000-11-29 2007-08-09 Goble E Marlowe Facet Joint Replacement
US7074237B2 (en) 2000-12-13 2006-07-11 Facet Solutions, Inc. Multiple facet joint replacement
US20030204259A1 (en) * 2000-12-13 2003-10-30 Goble E. Marlowe Multiple facet joint replacement
US7618455B2 (en) 2000-12-13 2009-11-17 Facet Solutions, Inc Multiple facet joint replacement
US7566345B1 (en) 2001-03-01 2009-07-28 Facet Solutions, Inc Prosthesis for the replacement of a posterior element of a vertebra
US20050234551A1 (en) * 2001-03-02 2005-10-20 Facet Solutions, Inc. Method and apparatus for spine joint replacement
US7090698B2 (en) 2001-03-02 2006-08-15 Facet Solutions Method and apparatus for spine joint replacement
US7445635B2 (en) 2001-03-02 2008-11-04 Facet Solutions Method and apparatus for spine joint replacement
US7955390B2 (en) 2001-03-02 2011-06-07 GME Delaware 2 LLC Method and apparatus for spine joint replacement
US8926700B2 (en) 2003-12-10 2015-01-06 Gmedelware 2 LLC Spinal facet joint implant
US20050131537A1 (en) * 2003-12-10 2005-06-16 Hoy Robert W. Spinal facet joint implant
US8419770B2 (en) 2003-12-10 2013-04-16 Gmedelaware 2 Llc Spinal facet implants with mating articulating bearing surface and methods of use
US20050131409A1 (en) * 2003-12-10 2005-06-16 Alan Chervitz Linked bilateral spinal facet implants and methods of use
US7588590B2 (en) 2003-12-10 2009-09-15 Facet Solutions, Inc Spinal facet implant with spherical implant apposition surface and bone bed and methods of use
US7753937B2 (en) 2003-12-10 2010-07-13 Facet Solutions Inc. Linked bilateral spinal facet implants and methods of use
US8579941B2 (en) 2004-02-17 2013-11-12 Alan Chervitz Linked bilateral spinal facet implants and methods of use
US7998177B2 (en) 2004-02-17 2011-08-16 Gmedelaware 2 Llc Linked bilateral spinal facet implants and methods of use
US8562649B2 (en) 2004-02-17 2013-10-22 Gmedelaware 2 Llc System and method for multiple level facet joint arthroplasty and fusion
US20070185492A1 (en) * 2004-02-17 2007-08-09 Alan Chervitz Linked Bilateral Spinal Facet Implants and Methods of Use
US8906063B2 (en) 2004-02-17 2014-12-09 Gmedelaware 2 Llc Spinal facet joint implant
US7914560B2 (en) 2004-02-17 2011-03-29 Gmedelaware 2 Llc Spinal facet implant with spherical implant apposition surface and bone bed and methods of use
US7998178B2 (en) 2004-02-17 2011-08-16 Gmedelaware 2 Llc Linked bilateral spinal facet implants and methods of use
US7588578B2 (en) 2004-06-02 2009-09-15 Facet Solutions, Inc Surgical measurement systems and methods
US7815648B2 (en) 2004-06-02 2010-10-19 Facet Solutions, Inc Surgical measurement systems and methods
US7507242B2 (en) 2004-06-02 2009-03-24 Facet Solutions Surgical measurement and resection framework
US8777994B2 (en) 2004-06-02 2014-07-15 Gmedelaware 2 Llc System and method for multiple level facet joint arthroplasty and fusion
US20060200149A1 (en) * 2005-02-22 2006-09-07 Hoy Robert W Polyaxial orhtopedic fastening apparatus
US20080167688A1 (en) * 2005-02-22 2008-07-10 Facet Solutions, Inc. Taper-Locking Fixation System
US7993373B2 (en) 2005-02-22 2011-08-09 Hoy Robert W Polyaxial orthopedic fastening apparatus
US8062336B2 (en) 2005-02-22 2011-11-22 Gmedelaware 2 Llc Polyaxial orthopedic fastening apparatus with independent locking modes
US8900273B2 (en) 2005-02-22 2014-12-02 Gmedelaware 2 Llc Taper-locking fixation system
US7722647B1 (en) 2005-03-14 2010-05-25 Facet Solutions, Inc. Apparatus and method for posterior vertebral stabilization
US8764801B2 (en) 2005-03-28 2014-07-01 Gmedelaware 2 Llc Facet joint implant crosslinking apparatus and method
US20060217718A1 (en) * 2005-03-28 2006-09-28 Facet Solutions, Inc. Facet joint implant crosslinking apparatus and method
US8308768B2 (en) 2007-01-10 2012-11-13 Gmedelaware 2 Llc System and method for facet joint replacement
US8252027B2 (en) 2007-01-10 2012-08-28 Gmedelaware 2 Llc System and method for facet joint replacement
US20080221622A1 (en) * 2007-01-10 2008-09-11 Facet Solutions, Inc. Facet Joint Replacement
US8206418B2 (en) 2007-01-10 2012-06-26 Gmedelaware 2 Llc System and method for facet joint replacement with detachable coupler
US8333789B2 (en) 2007-01-10 2012-12-18 Gmedelaware 2 Llc Facet joint replacement
US8211147B2 (en) 2007-01-10 2012-07-03 Gmedelaware 2 Llc System and method for facet joint replacement
US20090012566A1 (en) * 2007-01-10 2009-01-08 Facet Solutions, Inc. System and method for facet joint replacement
US8353933B2 (en) 2007-04-17 2013-01-15 Gmedelaware 2 Llc Facet joint replacement
US20080319489A1 (en) * 2007-04-17 2008-12-25 Facet Solutions, Inc. System and method for bone anchorage
US9050144B2 (en) 2007-04-17 2015-06-09 Gmedelaware 2 Llc System and method for implant anchorage with anti-rotation features
US8702759B2 (en) 2007-04-17 2014-04-22 Gmedelaware 2 Llc System and method for bone anchorage

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