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US5635250A Expired / Lapsed US ⏱️ 0.0 years remaining

Hydridosiloxanes as precursors to ceramic products

Assignee: SRI International Inc
•
Filing: 1995-05-09
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Granted: 1997-06-03
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Expires: 2015-05-09
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Abstract

Abstract A method is provided for preparing ceramic precursors from hydridosiloxane starting materials and then pyrolyzing these precursors to give rise to silicious ceramic materials. Si-H bonds present in the hydridosiloxane starting materials are catalytically activated, and the activated hydrogen atoms may then be replaced with nonhydrogen substituents. These preceramic materials are pyrolyzed in a selected atmosphere to give the desired ceramic product. Ceramic products which may be prepared by this technique include silica, silicon oxynitride, silicon carbide, metal silicates, and mullite.

Inventors

  • 👤 Yigal D. Blum
  • 👤 Sylvia M. Johnson
  • 👤 Michael I. Gusman

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-03 09:52
CPC Classifications
C; C04; C04B; C04B41/00; C04B41/009; C04B35/00; C04B35/01; C04B35/14; C04B35/16; C04B35/18; C04B35/185; C04B35/515; C04B35/56; C04B35/565; C04B35/571; C04B35/622; C04B35/626; C04B35/63; C04B35/632; C04B35/634; C04B41/45; C04B41/4505; C04B41/455; C04B41/4554; C04B41/80; C04B41/81; C08; C08G; C08G77/00; C08G77/04; C08G77/38; C08G77/382; C08G77/398; C08G77/48; C08G77/54; C08G79/00

Claims Analysis

Total Claims: 72
Claim 1
Independent Claim 217 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 2
Independent Claim 217 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 3
Dependent Claim 16 words
The method of claim 1, wherein curing is conducted using a compound capable of coupling hydridosiloxanes.
Claim 4
Dependent Claim 12 words
The method of claim 1, wherein R' is hydrogen or lower alkyl.
Claim 5
Dependent Claim 40 words
The method of claim 1, wherein in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 6
Dependent Claim 23 words
The method of claim 4, wherein the metal powder has an average particle size in the range of approximately 0.01 to 100 μm.
Claim 7
Dependent Claim 23 words
The method of claim 1, wherein in step (c) said ceramic precursor is admixed with both a metal powder and a ceramic powder.
Claim 8
Dependent Claim 20 words
The method of claim 6, wherein said metal powder is comprised of particulate aluminum and said ceramic material is mullite.
Claim 9
Dependent Claim 40 words
The method of claim 1, wherein in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 10
Dependent Claim 23 words
The method of claim 3, wherein the metal powder has an average particle size in the range of approximately 0.01 to 100 μm.
Claim 11
Dependent Claim 23 words
The method of claim 3, wherein in step (c) said ceramic precursor is admixed with both a metal powder and a ceramic powder.
Claim 12
Independent Claim 171 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 13
Independent Claim 171 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 14
Dependent Claim 40 words
The method of claim 11, wherein in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 15
Dependent Claim 23 words
The method of claim 11, wherein in step (c) said ceramic precursor is admixed with both a metal powder and a ceramic powder.
Claim 16
Independent Claim 178 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 17
Independent Claim 178 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 18
Dependent Claim 40 words
The method of claim 14, wherein in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 19
Dependent Claim 23 words
The method of claim 15, wherein in step (c) said ceramic precursor is admixed with both a metal powder and a ceramic powder.
Claim 20
Independent Claim 185 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 21
Independent Claim 185 words
A method for preparing a ceramic material, comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing said cured preceramic mixture at a temperature of at least about 500° C. to give said ceramic material.
Claim 22
Independent Claim 77 words
A method for preparing a ceramic material, comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both; and (d) pyrolyzing the mixture of step (c).
Claim 23
Independent Claim 77 words
A method for preparing a ceramic material, comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both; and (d) pyrolyzing the mixture of step (c).
Claim 24
Independent Claim 34 words
The method of any one of claims 1, 11, 14, 17 or 18, wherein, prior to conducting pyrolysis, the preceramic mixture is coated on a substrate, such that the ceramic material is a coating.
Claim 25
Independent Claim 35 words
The method of any one of claims 1, 11, 14, 17 or 18, wherein, prior to conducting pyrolysis, ceramic fibers are incorporated into the preceramic mixture, such that the ceramic material is a fiber-reinforced matrix.
Claim 26
Dependent Claim 220 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 27
Dependent Claim 220 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 28
Dependent Claim 24 words
The ceramic coating composition of claim 21, wherein the substrate is coated with the preceramic mixture after step (c) and prior to step (d).
Claim 29
Dependent Claim 20 words
The ceramic coating composition of claim 21, wherein the substrate is coated with the cured preceramic mixture after step (d).
Claim 30
Dependent Claim 18 words
The ceramic coating composition of claim 21, wherein, in the hydroxyl-containing compound, R' is hydrogen or lower alkyl.
Claim 31
Dependent Claim 41 words
The ceramic coating composition of 21, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 32
Dependent Claim 41 words
The ceramic coating composition of 21, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 33
Dependent Claim 174 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 34
Dependent Claim 174 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 35
Dependent Claim 24 words
The ceramic coating composition of claim 26, wherein the substrate is coated with the preceramic mixture after step (c) and prior to step (d).
Claim 36
Dependent Claim 20 words
The ceramic coating composition of claim 26, wherein the substrate is coated with the cured preceramic mixture after step (d).
Claim 37
Dependent Claim 41 words
The ceramic coating composition of 26, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 38
Dependent Claim 41 words
The ceramic coating composition of 26, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 39
Dependent Claim 181 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 40
Dependent Claim 181 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 41
Dependent Claim 24 words
The ceramic coating composition of claim 30, wherein the substrate is coated with the preceramic mixture after step (c) and prior to step (d).
Claim 42
Dependent Claim 20 words
The ceramic coating composition of claim 30, wherein the substrate is coated with the cured preceramic mixture after step (d).
Claim 43
Dependent Claim 29 words
The ceramic coating composition of claim 30, wherein, in the compound HNR" 2 , the R" moieties are independently selected from the group consisting of hydrogen and lower alkyl.
Claim 44
Dependent Claim 42 words
The ceramic coating composition of claim 30, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 45
Dependent Claim 188 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which Said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 46
Dependent Claim 188 words
A ceramic coating prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which Said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; and (e) pyrolyzing the preceramic mixture on a substrate, at a temperature of at least about 500° C., to provide a ceramic coating thereon.
Claim 47
Dependent Claim 24 words
The ceramic coating composition of claim 35, wherein the substrate is coated with the proceramic mixture after step (c) and prior to step (d).
Claim 48
Dependent Claim 20 words
The ceramic coating composition of claim 35, wherein the substrate is coated with the cured proceramic mixture after step (d).
Claim 49
Dependent Claim 42 words
The ceramic coating composition of claim 35, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 50
Dependent Claim 105 words
A ceramic coating composition prepared by the process comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both, to provide a preceramic mixture; (d) coating a substrate with the preceramic mixture, whereby a preceramic coating is provided; and (e) pyrolyzing the preceramic ceramic coating on the substrate, to provide a ceramic coating thereon.
Claim 51
Dependent Claim 105 words
A ceramic coating composition prepared by the process comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both, to provide a preceramic mixture; (d) coating a substrate with the preceramic mixture, whereby a preceramic coating is provided; and (e) pyrolyzing the preceramic ceramic coating on the substrate, to provide a ceramic coating thereon.
Claim 52
Dependent Claim 242 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 53
Dependent Claim 242 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a hydroxyl-containing compound of the formula R'--OH, wherein R' is (i) hydrogen, (ii) C 1 -C 10 alkyl or aryl of 1-2 rings, optionally substituted with hydroxyl, lower alkyl, halogeno, silyl, or amino groups, or combinations thereof, (iii) silyl optionally containing additional hydroxyl groups, or (iv) a metal optionally bound to one or more ligands and/or containing additional hydroxyl groups, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by oxygen-containing pendant groups OR' or oxygen-containing bridging moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 54
Dependent Claim 20 words
The ceramic matrix of claim 40, wherein the ceramic fibers are incorporated into the preceramic mixture prior to step (d).
Claim 55
Dependent Claim 18 words
The ceramic matrix composite of claim 40, wherein, in the hydroxyl-containing compound, R' is hydrogen or lower alkyl.
Claim 56
Dependent Claim 42 words
The ceramic matrix composite of claim 40, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 57
Dependent Claim 196 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 58
Dependent Claim 196 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing carbon-containing moieties into said hydridosiloxane starting material by reaction with a compound containing an unsaturated carbon-carbon bond, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane starting material have been replaced by pendant or bridging carbon-containing moieties; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds and unsaturated carbon-carbon bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 59
Dependent Claim 21 words
The ceramic matrix composite of claim 44, wherein the ceramic fibers are incorporated into the preceramic mixture prior to step (d).
Claim 60
Dependent Claim 42 words
The ceramic matrix composite of claim 44, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 61
Dependent Claim 202 words
A ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 62
Dependent Claim 202 words
A ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) introducing nitrogen-containing moieties into said starting material by reaction with a compound HNR" 2 wherein the R" are independently selected from hydrogen, lower alkyl, silyl, and aryl of 1-2 rings, to give a ceramic precursor in which hydrogen atoms in the hydridosiloxane polymer have been replaced with nitrogen-containing pendant or crosslinking groups; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 63
Dependent Claim 20 words
The ceramic matrix of claim 47, wherein the ceramic fibers are incorporated into the preceramic mixture prior to step (d).
Claim 64
Dependent Claim 29 words
The ceramic matrix composite of claim 47, wherein, in the compound HNR" 2 , the R" moieties are independently selected from the group consisting of hydrogen and lower alkyl.
Claim 65
Dependent Claim 42 words
The ceramic matrix composite of claim 47, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 66
Dependent Claim 210 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 67
Dependent Claim 210 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a hydridosiloxane starting material containing a plurality of Si--H bonds, and wherein at least about 20% of the silicon atoms present in the starting material have a hydrogen atom bound thereto; (b) reacting said hydridosiloxane starting material with a compound selected from the group consisting of ML a and L a M-OH, wherein M is a metal atom, L is an organic or inorganic ligand associated therewith, and a represents the molar ratio L/M, to give a ceramic precursor in which said activated Si--H bonds have been replaced by Si--M bonds; (c) adding a metal powder, a ceramic powder, or both, either prior to, during, or after step (b), wherein a catalyst effective to activate Si--H bonds is added in step (b), step (c) or both, such that a preceramic mixture is provided; (d) curing the preceramic mixture at a temperature between approximately 20° C. and 250° C., to provide a cured preceramic mixture; (e) incorporating ceramic fibers into the preceramic mixture, either prior to or during step (d), to provide a fiber-containing preceramic mixture; and (f) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 68
Dependent Claim 21 words
The ceramic matrix composite of claim 51, wherein the ceramic fibers are incorporated into the preceramic mixture prior to step (d).
Claim 69
Dependent Claim 42 words
The ceramic matrix composite of claim 51, wherein, in step (c), the ceramic precursor is admixed with a metal powder selected from the group consisting of aluminum, barium, boron, calcium, copper, hafnium, iron, magnesium, molybdenum, niobium, silicon, titanium, tungsten, yttrium and zirconium.
Claim 70
Dependent Claim 113 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both, to provide a preceramic mixture; (d) incorporating ceramic fibers into the preceramic mixture to provide a fiber-containing preceramic mixture; and (e) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 71
Dependent Claim 113 words
A fiber-reinforced ceramic matrix composite prepared by the process comprising: (a) providing a starting material comprising a silicon-containing polymer having a plurality of Si--H groups; (b) curing said silicon-containing polymer with light, by dehydrocoupling or by reaction with a coupling agent, to provide a ceramic precursor; (c) admixing (i) a catalyst effective to activate Si--H bonds, and (ii) a metal powder, with either the silicon-containing polymer, the ceramic precursor, or both, to provide a preceramic mixture; (d) incorporating ceramic fibers into the preceramic mixture to provide a fiber-containing preceramic mixture; and (e) pyrolyzing the fiber-containing preceramic mixture, at a temperature of at least about 500° C., to provide a fiber-reinforced ceramic matrix composite.
Claim 72
Dependent Claim 27 words
The method of claim 13, wherein, in the compound HNR" a , the R" moieties are independently selected from the group consisting of hydrogen and lower alkyl.

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