US4766013A
Expired / Lapsed
US
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Carbon composite article and method of making same
Assignee: 3M Co
•
Filing: 1984-06-04
•
Granted: 1988-08-23
•
Expires: 2004-06-04
Abstract
Abstract A composite structural ceramic article and method of fabrication thereof. The article of the invention is specifically designed for use in high temperature, corrosive and erosive environments such as those found in heat engines, heat exchangers, stationary power equipments and industrial process equipments. The article comprises a porous carbon fibrous substrate or other suitable high temperature fibrous substrate which may include: a pyrolytic carbon or appropriate chemical vapor deposited sheath formed about each fiber of the substrate; a chemically vapor deposited metallic carbide, oxide, boride or nitride coating over the coated fibers of the substrate; and an impermeable metallic carbide, oxide, boride or nitride outer protective layer formed about the entire periphery of the coated substrate. In accordance with the method of the invention, the metallic coating is applied to the fibers in such a manner such that internal porosity of the article is precisely controlled and a flaw resistant, tough, non-catastrophic failing structural ceramic body is formed.
Inventors
- 👤 James W. Warren
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 14:42
CPC Classifications
F; F16; F16D; F16D69/00; F16D69/02; F16D69/023; C; C04; C04B; C04B35/00; C04B35/01; C04B35/14; C04B35/515; C04B35/56; C04B35/565; C04B35/58; C04B35/5805; C04B35/58064; C04B35/58071; C04B35/584; C04B35/622; C04B35/626; C04B35/628; C04B35/62844; C04B35/62847; C04B35/62849; C04B35/62857; C04B35/6286; C04B35/62863; C04B35/62865; C04B35/62871; C04B35/62873; C04B35/62876; C04B35/62894; C04B35/71; C04B35/78; C04B35/80; C04B35/83; C22; C22C; C22C49/00; C22C49/02; C22C49/10; C04B2235/00; C04B2235/02; C04B2235/50; C04B2235/52; C04B2235/5208; C04B2235/5216; C04B2235/522; C04B2235/5224; C04B2235/5228; C04B2235/5232; C04B2235/524; C04B2235/5244; C04B2235/5248; C04B2235/60; C04B2235/608; C04B2235/612; C04B2235/614; C04B2235/70; C04B2235/74; C04B2235/77; Y; Y10; Y10T; Y10T428/00; Y10T428/29; Y10T428/2913; Y10T428/2918; Y10T428/30
Claims Analysis
Total Claims: 103
Claim 1
Independent Claim
203 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers selected from a group consisting of pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, exposing said starting substrate to an elevated temperature of about 1800° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shape desired of the end product composite article, supporting said shaped substrate in a second controlled environment while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said shaped substrate through chemical vapor deposition a metal capable of reacting with carbon, oxygen, boron and nitrogen to form a carbide, oxide, boride and nitride.
Claim 2
Independent Claim
203 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers selected from a group consisting of pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, exposing said starting substrate to an elevated temperature of about 1800° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shape desired of the end product composite article, supporting said shaped substrate in a second controlled environment while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said shaped substrate through chemical vapor deposition a metal capable of reacting with carbon, oxygen, boron and nitrogen to form a carbide, oxide, boride and nitride.
Claim 3
Dependent Claim
107 words
A method of making a composite article as defined in claim 1 including the step of removing said chemical vapor deposition coated article from said second controlled environment, placing it in a third controlled environment, and heating said article to a temperature of between approximately 1800° F. and approximately 3200° F., and exposing said article to a halide gas containing carbon and silicon selected from a group consisting of methyl trichlorosilane, dimethyldichlorosilane, silicon tetrachloride, trimethylchlorosilane, dichlorosilane, silicon dichloride, silicon tetrabromide, tribromosilane, dibromosilane and silicon dibromide to form a uniform chemical vapor deposition coating of silicon carbide over the coated fibers and periphery of said diffusion coated article.
Claim 4
Dependent Claim
57 words
A method of making a composite article as defined in claim 1 in which said chemical vapor deposition coated article is formed by placing said shaped substrate into a controlled deposition environment, continuously varying the pressure within said environment, and depositing on the fibers of said shaped substrate a coating of silicon carbide of a predetermined thickness.
Claim 5
Dependent Claim
32 words
A method of making a composite article as defined in claim 1 in which said coated article is formed by depositing said coating into said shaped substrate fabricated from silicon carbide fibers.
Claim 6
Dependent Claim
38 words
A method of making a composite article as defined in claim 1 including the step of removing said coated article from said second controlled environment and controllably introducing a metal oxide into the pores of said coated article.
Claim 7
Dependent Claim
57 words
A method of making a composite article as defined in claim 3 in which said coated article is formed by maintaining said shaped substrate in the presence of a gas containing silicon at a temperature greater than about 1700° F. to deposit a coating of silicon carbide over the coated fibers and periphery of said shaped substrate.
Claim 8
Dependent Claim
32 words
A method of making a composite article as defined in claim 1 in which said hydrocarbon gas is selected from a group consisting of methane, propane, ethane, butane, ethylene, acetylene and benzine.
Claim 9
Dependent Claim
36 words
A method of making a composite article as defined in claim 1 in which said multiplicity of carbon fibers are formed into a starting substrate having a fiber volume of between about 5% and about 65%.
Claim 10
Independent Claim
260 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers, exposing said starting substrate to an elevated temperature of between about 1000° F. and about 1800° F. for a period of time of between about 1 hour and about 100 hours, suspending said starting substrate within a first vacuum pressure controlled environment, forming an intermediate substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shaped desired of the end product composite article, supporting said shaped substrate in a second controlled environment while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., forming a coated article by depositing about said fibers of said shaped substrate, through chemical vapor deposition, a silicon metal capable of reacting with carbon to form silicon carbide, removing said diffusion coated article from said second controlled environment, heating said article within a controlled environment to a temperature of between approximately 1350° F. and approximately 2500° F., and exposing said article to a gas containing carbon and silicon to form a uniform chemical vapor deposition coating of silicon carbide over the coated fibers, the fiber interstices, and the periphery of said diffusion coated article.
Claim 11
Independent Claim
260 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers, exposing said starting substrate to an elevated temperature of between about 1000° F. and about 1800° F. for a period of time of between about 1 hour and about 100 hours, suspending said starting substrate within a first vacuum pressure controlled environment, forming an intermediate substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shaped desired of the end product composite article, supporting said shaped substrate in a second controlled environment while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., forming a coated article by depositing about said fibers of said shaped substrate, through chemical vapor deposition, a silicon metal capable of reacting with carbon to form silicon carbide, removing said diffusion coated article from said second controlled environment, heating said article within a controlled environment to a temperature of between approximately 1350° F. and approximately 2500° F., and exposing said article to a gas containing carbon and silicon to form a uniform chemical vapor deposition coating of silicon carbide over the coated fibers, the fiber interstices, and the periphery of said diffusion coated article.
Claim 12
Dependent Claim
29 words
A method of making a composite article as defined in claim 9 in which the pressure within the second controlled environment is fluctuated from approximately 0.01 to 0.6 atmospheres.
Claim 13
Dependent Claim
36 words
A method of making a composite article as defined in claim 9 in which said multiplicity of high temperature resistant fibers is in the form of a felt material having a multiplicity of randomly oriented fibers.
Claim 14
Dependent Claim
36 words
A method of making a composite article as defined in claim 9 in which said multiplicity of high temperature resistant fibers is in the form of a macerated material having a multiplicity of randomly oriented fibers.
Claim 15
Dependent Claim
35 words
A method of making a composite article as defined in claim 9 in which said multiplicity of high temperature resistant fibers is in the form of a mascerated material having a multiplicity of chopped fibers.
Claim 16
Dependent Claim
32 words
A method of making a composite article as defined in claim 9 in which said multiplicity of high temperature resistant fibers is in the form of a woven material having interwoven fibers.
Claim 17
Dependent Claim
33 words
A method of making a composite article as defined in claim 9 in which said multiplicity of high temperature resistant fibers is in the form of a tape material having interwoven carbon fibers.
Claim 18
Independent Claim
341 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers in the form of a woven material having a multiplicity of interwoven fibers said fibers being selected from a group consisting of ceramic matrial, pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, suspending said starting substrate within a first controlled environment, forming an intermediate substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas selected from a group consisting of methane, propane, ethane, butane, ethylene, acetylene and benzine to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shape desired of the end product composite article, supporting said shaped substrate in a second controlled environment at less than atmospheric pressure while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., forming a coated article by depositing about said fibers of said shaped substrate, through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron and nitrogen, said metal being selected from a group consisting of silicon, boron, aluminum, magnesium, tantalum, hafnium, titanium, berillium, thorium and zirconium, removing said article from said second controlled environment and suspending it thereabove while maintaining said at a temperature of on the order of 3200° F. for about fifteen minutes, removing said coated article from said second controlled environment, heating said article within a controlled environment to a temperature of between approximately 1350° F. and approximately 2500° F., and exposing said article to a halide gas containing carbon and silicon selected from a group consisting of dimethyldichlorosilane, silicon tetrachloride trichlorosilane, dichlorosilane silicon dichloride, silicon tetrabromide, tribromosilane, dibromosilane and silicon dibromide to form a uniform chemical vapor deposition coating of silicon carbide over the coated fibers and periphery of said diffusion coated article.
Claim 19
Independent Claim
341 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers in the form of a woven material having a multiplicity of interwoven fibers said fibers being selected from a group consisting of ceramic matrial, pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, suspending said starting substrate within a first controlled environment, forming an intermediate substrate by heating said starting substrate to a temperature of between approximately 1500° F. and approximately 4200° F. while exposing said starting substrate to a hydrocarbon gas selected from a group consisting of methane, propane, ethane, butane, ethylene, acetylene and benzine to form a uniform layer of pyrolytic carbon about each of the fibers in said starting substrate, removing said intermediate substrate from said first controlled environment and forming it into a shaped substrate having the approximate shape desired of the end product composite article, supporting said shaped substrate in a second controlled environment at less than atmospheric pressure while heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., forming a coated article by depositing about said fibers of said shaped substrate, through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron and nitrogen, said metal being selected from a group consisting of silicon, boron, aluminum, magnesium, tantalum, hafnium, titanium, berillium, thorium and zirconium, removing said article from said second controlled environment and suspending it thereabove while maintaining said at a temperature of on the order of 3200° F. for about fifteen minutes, removing said coated article from said second controlled environment, heating said article within a controlled environment to a temperature of between approximately 1350° F. and approximately 2500° F., and exposing said article to a halide gas containing carbon and silicon selected from a group consisting of dimethyldichlorosilane, silicon tetrachloride trichlorosilane, dichlorosilane silicon dichloride, silicon tetrabromide, tribromosilane, dibromosilane and silicon dibromide to form a uniform chemical vapor deposition coating of silicon carbide over the coated fibers and periphery of said diffusion coated article.
Claim 20
Dependent Claim
71 words
A carbon-silicon composite article comprising a multiplicity of carbon fibers forming a shaped article, a coating of pyrolytic carbon extending over each of said fibers, a chemical vapor deposition formed coating of silicon carbide extending over each of said pyrolytic carbon coated fibers, said pyrolytic carbon coating and said silicon coating having been applied to said fibers in a manner whereby said fibers are free to move relative to said coatings.
Claim 21
Dependent Claim
71 words
A carbon-silicon composite article comprising a multiplicity of carbon fibers forming a shaped article, a coating of pyrolytic carbon extending over each of said fibers, a chemical vapor deposition formed coating of silicon carbide extending over each of said pyrolytic carbon coated fibers, said pyrolytic carbon coating and said silicon coating having been applied to said fibers in a manner whereby said fibers are free to move relative to said coatings.
Claim 22
Dependent Claim
22 words
A carbon-silicon composite article as defined in claim 19 in which said chemical vapor deposition formed diffusion coating consists of silicon carbide.
Claim 23
Dependent Claim
22 words
A carbon-silicon composite article as defined in claim 17 in which said chemical vapor deposition formed diffusion coating consists of silicon nitride.
Claim 24
Dependent Claim
22 words
A carbon-silicon composite article as defined in claim 17 in which said chemical vapor deposition formed diffusion coating consists of silicon oxide.
Claim 25
Dependent Claim
23 words
A carbon-silicon composite article as defined in claim 17 in which said chemical vapor deposition formed diffusion coating consists of hafnium 10 tantalum.
Claim 26
Dependent Claim
22 words
A carbon-silicon composite article as defined in claim 17 in which said chemical vapor deposition formed diffusion coating consists of titanium diboride.
Claim 27
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said chemical vapor deposition formed diffusion coating consists of tungsten.
Claim 28
Dependent Claim
30 words
A carbon-silicon composite article as defined in claim 19 in which silicon nitride extends substantially over each of said coated fibers and substantially over the outer periphery of said article.
Claim 29
Dependent Claim
30 words
A carbon-silicon composite article as defined in claim 20 in which silicon oxide extends substantially over each of said coated fibers and substantially over the outer periphery of said article.
Claim 30
Dependent Claim
36 words
A carbon-silicon composite article as defined in claim 17 in which a coating of chemical vapor deposited silicon carbide extends substantially over each of said coated fibers and substantially over the outer periphery of said article.
Claim 31
Dependent Claim
23 words
A carbon-silicon composite article as defined in claim 17 in which the carbon fibers and silicon coating have different coefficients of thermal expansion.
Claim 32
Dependent Claim
22 words
A carbon-silicon composite article as defined in claim 17 whereby the density of said article is between 0.3 gm/cc and 4.0 gm/cc.
Claim 33
Dependent Claim
15 words
A carbon-silicon composite article as defined in claim 17 wherein said composite article is anisotropic.
Claim 34
Dependent Claim
34 words
A carbon-silicon composite article as defined in claim 17 wherein said multiplicity of carbon fibers forming the shaped article are in the form of a woven material having a multiplicity of interwoven carbon fibers.
Claim 35
Dependent Claim
34 words
A carbon-silicon composite article as defined in claim 17 wherein said multiplicity of carbon fibers forming the shape article are in the form of a felt material having a multiplicity of randomly oriented fibers.
Claim 36
Dependent Claim
34 words
A carbon-silicon composite article as defined in claim 17 wherein said multiplicity of carbon fibers forming the shaped article are in the form of a mascerated material having a multiplicity of randomly oriented fibers.
Claim 37
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are pyrolyzed rayon.
Claim 38
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are pyrolyzed polyacrylonitrile.
Claim 39
Dependent Claim
20 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are wool.
Claim 40
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are pitch fibers.
Claim 41
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are silicon carbide.
Claim 42
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are silicon nitride.
Claim 43
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are boron nitride.
Claim 44
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are aluminum oxide.
Claim 45
Dependent Claim
21 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are silicon oxide.
Claim 46
Dependent Claim
20 words
A carbon-silicon composite article as defined in claim 17 in which said carbon fibers forming said shaped article are aluminosilicate.
Claim 47
Dependent Claim
54 words
A carbon-silicon composite article comprising a multiplicity of carbon fibers forming a shaped article, a coating of silicon carbide formed by chemical vapor deposition extending over each of said fibers, said silicon carbide coating having been applied to said fibers in a manner whereby said fibers are free to move relative to said coatings.
Claim 48
Dependent Claim
54 words
A carbon-silicon composite article comprising a multiplicity of carbon fibers forming a shaped article, a coating of silicon carbide formed by chemical vapor deposition extending over each of said fibers, said silicon carbide coating having been applied to said fibers in a manner whereby said fibers are free to move relative to said coatings.
Claim 49
Dependent Claim
46 words
A carbon-silicon composite article as defined in claim 43 including a chemical vapor deposition formed coating of silicon carbide extending over each of said pyrolytic silicon carbide coatings having been applied in a manner whereby said fibers are free to move relative to both said coatings.
Claim 50
Independent Claim
130 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers selected from a group consisting of ceramic, pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, exposing said starting substrate to an elevated temperature of about 1800° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate within a controlled environment, heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said starting substrate through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron, silicon and nitrogen to form a carbide, oxide, boride, silicide and nitride.
Claim 51
Independent Claim
130 words
A method of making a composite article comprising the steps of: forming a starting substrate from a multiplicity of high temperature resistant fibers selected from a group consisting of ceramic, pyrolyzed wool, rayon, polyacrylonitrile and pitch fibers, exposing said starting substrate to an elevated temperature of about 1800° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate within a controlled environment, heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said starting substrate through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron, silicon and nitrogen to form a carbide, oxide, boride, silicide and nitride.
Claim 52
Dependent Claim
20 words
A method as defined in claim 45 in which said starting substrate includes granular silicon carbide intermixed with said fibers.
Claim 53
Dependent Claim
19 words
A method as defined in claim 45 in which said starting substrate includes granular graphite intermixed with said fibers.
Claim 54
Independent Claim
122 words
A method of making a composite article comprising the steps of: forming a starting substrate from a granular material selected from a group consisting of silicon carbide and graphite, exposing said starting substrate to an elevated temperature of about 1600°-2200° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate within a controlled environment, heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said starting substrate through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron, silicon and nitrogen to form a carbide, oxide, boride, silicide and nitride.
Claim 55
Independent Claim
122 words
A method of making a composite article comprising the steps of: forming a starting substrate from a granular material selected from a group consisting of silicon carbide and graphite, exposing said starting substrate to an elevated temperature of about 1600°-2200° F. for a period of time sufficient to thermally stabilize said substrate, suspending said starting substrate within a controlled environment, heating said shaped substrate to a temperature of between approximately 1350° F. and approximately 2500° F., and forming a coated article having a controlled degree of open porosity by depositing about said fibers of said starting substrate through chemical vapor deposition, a metal capable of reacting with carbon, oxygen, boron, silicon and nitrogen to form a carbide, oxide, boride, silicide and nitride.
Claim 56
Dependent Claim
97 words
In combination, a substrate formed from a plurality of discrete elements defining a porours relationship, the substrate having anisotropic properites and having a first coefficient of thermal expansion, and a matrix disposed on the substrate and having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and freely movable relative to the substrate to accommodate the different coefficients of thermal expansion of the substrate and the matrix, the matrix being formed from a first material including a first element having refractory properties and a second element chemically bound to the first element.
Claim 57
Dependent Claim
97 words
In combination, a substrate formed from a plurality of discrete elements defining a porours relationship, the substrate having anisotropic properites and having a first coefficient of thermal expansion, and a matrix disposed on the substrate and having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and freely movable relative to the substrate to accommodate the different coefficients of thermal expansion of the substrate and the matrix, the matrix being formed from a first material including a first element having refractory properties and a second element chemically bound to the first element.
Claim 58
Dependent Claim
25 words
The combination set forth in claim 49 wherein the discrete members in the plurality define interstices and wherein the matrix is disposed in such interstices.
Claim 59
Dependent Claim
16 words
The combination set forth in claim 49 wherein the matrix is disposed directly on the substrate.
Claim 60
Dependent Claim
21 words
The combination set forth in claim 49 wherein the matrix is permeable and an impermeable layer is disposed on the matrix.
Claim 61
Dependent Claim
47 words
The combination set forth in claim 49 wherein the substrate is formed from discrete elements of a material containing carbon and the matrix is formed from a material selected from the group consisting of silicon carbide, silicon nitride, silicon oxide, hafnium 10 tantalum, titanium diboride and tungsten.
Claim 62
Dependent Claim
29 words
The combination set forth in claim 39 wherein the substrate is formed from a material selected from the group consisting of ceramic, pyrolized wool, rayon, polyacrylonitrile and pitch fibers.
Claim 63
Dependent Claim
31 words
The combination set forth in claim 54 wherein a material selected from the group consisting of granular silicon carbide and granular graphite is mixed with the other materials in the substrate.
Claim 64
Dependent Claim
133 words
In combination, a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements defining a porous relationship and defining interstices between the discrete elements, means disposed on the substrate at the interstices of the substrate for promoting a load transfer throughout the substrate, and a matrix disposed on the promoting means at the interstices and having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and freely movable relative to the substrate for providing for changes in the relative positions of the substrate and the matrix in accordance with changes in stresses on the substrate and the matrix, the matrix being formed from a material including a first element having refractory properties and a second element chemically bound to the first element.
Claim 65
Dependent Claim
133 words
In combination, a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements defining a porous relationship and defining interstices between the discrete elements, means disposed on the substrate at the interstices of the substrate for promoting a load transfer throughout the substrate, and a matrix disposed on the promoting means at the interstices and having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and freely movable relative to the substrate for providing for changes in the relative positions of the substrate and the matrix in accordance with changes in stresses on the substrate and the matrix, the matrix being formed from a material including a first element having refractory properties and a second element chemically bound to the first element.
Claim 66
Dependent Claim
15 words
The combination set forth in claim 56 wherein the promoting means constitutes a pyrolyzed binder.
Claim 67
Dependent Claim
43 words
The combination set forth in claim 56 wherein the promoting means constitutes a pyrolyzed carbon and the matrix constitutes a deposition of a material selected from a group consisting of silicon carbide, silicon nitride, silicon oxide, hafnium 10 tantalum, titanium diboride and tungsten.
Claim 68
Dependent Claim
23 words
The combination set forth in claim 56 wherein the matrix is permeable and porous and an impermeable layer is disposed on the matrix.
Claim 69
Dependent Claim
55 words
The combination set forth in claim 56 wherein the substrate is formed from discrete elements of a material containing carbon, the load-distributing means is formed from pyrolyzed carbon and the matrix is formed from a material selected from the group consisting of silicon carbide, silicon nitride, silicon oxide, hafnium 10, tantalum, titanium diboride and tungsten.
Claim 70
Dependent Claim
36 words
The combination set forth in claim 60 wherein the matrix is pervious and porous and an impermeable layer selected from a group consisting of silicon nitride, silicon carbide and silicon oxide is disposed on the matrix.
Claim 71
Dependent Claim
17 words
The combination set forth in claim 56 wherein the discrete elements have a fibrous or granular construction.
Claim 72
Dependent Claim
29 words
The combination set forth in claim 62 wherein the substrate is formed from a material selected from the group consisting of ceramic, pyrolized wool, rayon, polyacrylonitrile and pitch fibers.
Claim 73
Dependent Claim
30 words
The combination set forth in claim 63 wherein a material selected from the group consisting of silicon carbide and granular graphite is mixed in the substrate with the other material.
Claim 74
Independent Claim
114 words
A method of forming a refractory composite material, including the steps of: providing a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements, producing a layer of pyrolyzed material on the discrete members of the substrate, and producing on the pyrolyzed material a chemical vapor deposition of a material having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and defining a matrix freely movable relative to the pyrolized material and the substrate, the matrix being formed from a first element having refractory properties and providing a positive ionization and a material providing a negative ionization and bound to the first element.
Claim 75
Independent Claim
114 words
A method of forming a refractory composite material, including the steps of: providing a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements, producing a layer of pyrolyzed material on the discrete members of the substrate, and producing on the pyrolyzed material a chemical vapor deposition of a material having a second coefficient of thermal expansion different from the first coefficient of thermal expansion and defining a matrix freely movable relative to the pyrolized material and the substrate, the matrix being formed from a first element having refractory properties and providing a positive ionization and a material providing a negative ionization and bound to the first element.
Claim 76
Dependent Claim
33 words
The method set forth in claim 65 wherein the substrate is porous and the matrix is porous and permeable and wherein a chemical vapor deposition having impermeable characteristics is provided on the matrix.
Claim 77
Dependent Claim
41 words
The method set forth in claim 65 wherein the layer of the pyrolyzed material on the discrete members of the substrate is provided by: coating a binder on the discrete elements of the substrate and pyrolyzing the binder after such coating.
Claim 78
Dependent Claim
43 words
The method set forth in claim 67 wherein the discrete elements in the substrate define interstices and wherein the pyrolyzed binder is disposed at the interstices defined by the discrete elements and the matrix is disposed on the discrete elements at the interstices.
Claim 79
Dependent Claim
31 words
The method set forth in claim 65 wherein the layer of the pyrolyzed material on the substrate is formed by depositing the pyrolyzed material on the discrete elements of the substrate.
Claim 80
Dependent Claim
27 words
The method set forth in claim 69 wherein the pyrolyzed material deposited on the discrete elements encase the discrete elements and the matrix encases the pyrolyzed material.
Claim 81
Dependent Claim
39 words
The method set forth in claim 65 wherein the chemical vapor deposition is obtained from a material selected from the group consisting of methyltrichlorosilane, dimethyl dichlorosilane, trimethylchlorosilane, dichlorosilane, silicon tetrachloride, silicon dichloride, silicon tetrabromide, triborosilane, dibromosilane and silicon dibromide.
Claim 82
Dependent Claim
35 words
The method set forth in claim 71 wherein the pyrolized material deposited on the discrete elements is obtained from a gas selected from the group consisting of methane, propane, ethane, butane, ethylene, acetylene and benzene.
Claim 83
Dependent Claim
29 words
The method set forth in claim 68 wherein the pyrolized binder disposed on the interstices is obtained by coating the discrete elements with a binder and pyrolizing the binder.
Claim 84
Independent Claim
100 words
A method of forming a refractory composite material, including the steps of: providing a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements and having porous characteristics, disposing the substrate in a particular shape, and producing on the substrate a chemical vapor deposition of a material having a second coefficient of thermal expansion different from the first coefficient of the thermal expansion and defining a matrix freely movable relative to the substrate, the matrix being formed from a first element having refractory properties and a second element chemically bound to the first element.
Claim 85
Independent Claim
100 words
A method of forming a refractory composite material, including the steps of: providing a substrate having a first coefficient of thermal expansion and formed from a plurality of discrete elements and having porous characteristics, disposing the substrate in a particular shape, and producing on the substrate a chemical vapor deposition of a material having a second coefficient of thermal expansion different from the first coefficient of the thermal expansion and defining a matrix freely movable relative to the substrate, the matrix being formed from a first element having refractory properties and a second element chemically bound to the first element.
Claim 86
Dependent Claim
33 words
A method as set forth in claim 74 wherein the chemical vapor deposition is provided with permeable characteristics and a chemical vapor deposition of an impermeable material is produced on the pervious deposition.
Claim 87
Dependent Claim
35 words
A method as set forth in claim 74 wherein the matrix is formed from a material selected from the group consisting of silicon carbide, silicon nitride, silicon oxide, hafnium 10, tantalum, titanium diboride and tungsten.
Claim 88
Dependent Claim
57 words
A method as set forth in claim 75 wherein the matrix is formed from a material selected from a group consisting of silicon carbide, silicon nitride, silicon oxide, hafnium 10 tantalum, titanium diboride and tungsten and the impermeable layer is formed from a material selected from a group consisting of silicon carbide, silicon nitride and silicon oxide.
Claim 89
Dependent Claim
39 words
The method set forth in claim 77 wherein the chemical vapor deposition is obtained from a material selected from the group consisting of methyltrichlorosilane, dimethyl dichlorosilane, trimethylchlorosilane, dichlorosilane, silicon tetrachloride, silicon dichloride, silicon tetrabromide, triborosilane, dibromosilane and silicon dibromide.
Claim 90
Independent Claim
105 words
A method of forming a refractory composite material, including the steps of: providing a plurality of discrete elements in the form of a substrate, the discrete elements having a first coefficient of thermal expansion, compressing the substrate formed from the discrete elements, heating the substrate, and passing gases through the heated substrate to apply to the substrate a matrix having a different coefficient of thermal expansion than that of the substrate and providing for a free movement of the matrix relative to the substrate, the matrix being formed from a first element having refractory properties and a second element chemically bound to the first element.
Claim 91
Independent Claim
105 words
A method of forming a refractory composite material, including the steps of: providing a plurality of discrete elements in the form of a substrate, the discrete elements having a first coefficient of thermal expansion, compressing the substrate formed from the discrete elements, heating the substrate, and passing gases through the heated substrate to apply to the substrate a matrix having a different coefficient of thermal expansion than that of the substrate and providing for a free movement of the matrix relative to the substrate, the matrix being formed from a first element having refractory properties and a second element chemically bound to the first element.
Claim 92
Dependent Claim
24 words
A method as set forth in claim 79 wherein the substrate is formed with porous characteristics and the matrix is formed with porous characteristics.
Claim 93
Dependent Claim
21 words
A method as set forth in claim 80 wherein the substrate is shaped before the matrix is applied to the substrate.
Claim 94
Dependent Claim
19 words
A method as set forth in claim 81 wherein the discrete elements constitute fibers disposed in an anisotropic relationship.
Claim 95
Dependent Claim
18 words
A method as set forth in claim 80 wherein a hard, impermeable coating is applied on the matrix.
Claim 96
Dependent Claim
14 words
A method as set forth in claim 83 wherein the discrete elements constitute grains.
Claim 97
Dependent Claim
47 words
A method as set forth in claim 80 wherein the matrix is permeable and the combination of the substrate and the matrix is heated and gases are passed through the heated combination of the substrate and the matrix to produce a hard, impermeable coating on the matrix.
Claim 98
Dependent Claim
29 words
A method as set forth in claim 79 wherein a material promoting a load transfer is deposited on the substrate before the deposition of the matrix on the substrate.
Claim 99
Dependent Claim
38 words
A method as set forth in claim 86 wherein the material promoting the load transfer is deposited by passing through the substrate a gas selected from a group consisting of methane, propane, ethane, butane, ethylene, acetylene and benzene.
Claim 100
Dependent Claim
34 words
A method as set forth in claim 87 wherein the material promoting the load transfer encases the discrete elements and wherein the matrix is deposited by chemical vapor deposition to encase the discrete elements.
Claim 101
Dependent Claim
30 words
A method as set forth in claim 87 wherein the material promoting the load transfer is deposited by coating the discrete elements with a binder and the binder is pyrolized.
Claim 102
Dependent Claim
40 words
A method as set forth in claim 89 wherein the material promoting the load transfer is disposed in the interstices between the discrete elements and the matrix is deposited by chemical vapor deposition at the interstices between the discrete elements.
Claim 103
Dependent Claim
21 words
A method as set forth in claim 79 wherein a variable pressure is applied to the gases passing through the substrate.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1991-08-23 | 1992-02-22 | 1992-08-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1995-08-23 | 1996-02-22 | 1996-08-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1999-08-23 | 2000-02-22 | 2000-08-23 | $7700.00 | Window Closed / Lapsed |