US5225283A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Coating for protecting a carbon-carbon composite from oxidative degradation
Assignee: BABB HENRY C JR AS ATTORNEY AND PROXY
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Filing: 1987-04-24
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Granted: 1993-07-06
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Expires: 2007-04-24
Abstract
Abstract A process for forming a high temperature oxidation resistant coating on a carbon-carbon composite is disclosed and claimed. The process comprises applying a cyclosiloxane monomer blend containing a filler such as silicon carbide to a carbon-carbon composite, polymerizing and pyrolyzing said blend to form a filled black glass protective coating on the carbon-carbon composite.
Inventors
- 👤 Roger Y. Leung
- 👤 Bryan A. Weyneth
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 16:06
CPC Classifications
C; C04; C04B; C04B41/00; C04B41/009; C03; C03C; C03C14/00; C03C14/004; C04B41/45; C04B41/4505; C04B41/455; C04B41/4554; C04B41/50; C04B41/5022; C04B41/80; C04B41/81; C04B41/85; C04B41/86; C09; C09D; C09D183/00; C09D183/04; C03C2214/00; C03C2214/04; C04B2111/00; C04B2111/00474; C04B2111/00482; C04B2111/00568; Y; Y10; Y10T; Y10T428/00; Y10T428/30
Claims Analysis
Total Claims: 31
Claim 1
Independent Claim
298 words
A method of forming a high temperature oxidation resistant coating on a carbon-carbon composite comprising the steps: (a) polymerizing a blend of a hydrosilylation catalyst, a filler and 1) a cyclosiloxane monomer of formula ##STR3## where n is an integer from 3 to about 20, R is hydrogen, and R' is an alkene having from 2 to about 20 carbon atoms and containing a vinyl-silicon bond, or 2) at least two different cyclosiloxane monomers of the same formula as above and with the same n integer value range where R' is an alkyl group of from 1 to about 20 carbon atoms and in one cyclosiloxane monomer R is hydrogen, and in the others R is an alkene of from 2 to about 20 carbon atoms containing a vinyl-silicon bond to produce a black glass precursor polymer containing a filler; (b) pyrolyzing said polymer precursor under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to form a black glass powder containing a filler; (c) reducing the particle size of the filled black glass powder; (d) mixing said reduced particle size black glass with a new portion of the blend of the cyclosiloxane monomers and hydrosilylation catalyst and optionally a filler of step (a) to form a slurry; (e) applying said slurry from step (d) to a carbon-carbon composite; (f) curing said coated carbon-carbon composite at curing conditions to produce a cyclosiloxane polymer coated carbon-carbon composite; (g) pyrolyzing said filled polymer coated carbon-carbon composite under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to produce a filled black glass containing coating on said carbon-carbon composite; and (h) recovering said filled black glass coated carbon-carbon composite.
Claim 2
Independent Claim
298 words
A method of forming a high temperature oxidation resistant coating on a carbon-carbon composite comprising the steps: (a) polymerizing a blend of a hydrosilylation catalyst, a filler and 1) a cyclosiloxane monomer of formula ##STR3## where n is an integer from 3 to about 20, R is hydrogen, and R' is an alkene having from 2 to about 20 carbon atoms and containing a vinyl-silicon bond, or 2) at least two different cyclosiloxane monomers of the same formula as above and with the same n integer value range where R' is an alkyl group of from 1 to about 20 carbon atoms and in one cyclosiloxane monomer R is hydrogen, and in the others R is an alkene of from 2 to about 20 carbon atoms containing a vinyl-silicon bond to produce a black glass precursor polymer containing a filler; (b) pyrolyzing said polymer precursor under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to form a black glass powder containing a filler; (c) reducing the particle size of the filled black glass powder; (d) mixing said reduced particle size black glass with a new portion of the blend of the cyclosiloxane monomers and hydrosilylation catalyst and optionally a filler of step (a) to form a slurry; (e) applying said slurry from step (d) to a carbon-carbon composite; (f) curing said coated carbon-carbon composite at curing conditions to produce a cyclosiloxane polymer coated carbon-carbon composite; (g) pyrolyzing said filled polymer coated carbon-carbon composite under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to produce a filled black glass containing coating on said carbon-carbon composite; and (h) recovering said filled black glass coated carbon-carbon composite.
Claim 3
Dependent Claim
49 words
The process of claim 1 where said filled black glass coated carbon-carbon composite is further impregnated with the blend of step (a), and pyrolyzed as in claim 1 to produce a crack-free filled black glass coating on said carbon-carbon composite and recovering said filled black glass coated carbon-carbon composite.
Claim 4
Dependent Claim
27 words
The process of claim 1 where said filler is selected from the group consisting of silicon carbide, silicon nitride, titania, hafnia, zirconia, silica, alumina and mixtures thereof.
Claim 5
Dependent Claim
15 words
The process of claim 3 where the filler is a powder, whisker, or a fiber.
Claim 6
Dependent Claim
54 words
The process of claim 3 where said black glass containing filler has an amount of filler present in the range of from about 20% to about 70% in step (b) of claim 1 and said coating has an amount of filler in the range of from 15% to about 65% in said coated composite.
Claim 7
Dependent Claim
40 words
The process of claim 2 where said impregnation is applied under a reduced pressure in the range from about 1 mm Hg to about 29 mm Hg and for a time in the range of 1 minute to 60 minutes.
Claim 8
Dependent Claim
54 words
The process of claim 1 where said polymerization takes place at a temperature in the range of from about 25° C. to about 300° C., a pressure in the range of from about 14 psi to about 30,000 psi, and a time in the range of from about 1 minute to about 600 minutes.
Claim 9
Dependent Claim
26 words
The process of claim 1 where said filled black glass is present in said monomer mixture of step (d) at from about 20% to about 70%.
Claim 10
Dependent Claim
24 words
The process of claim 1 where said coating comprises an amount of black glass in the range of from about 35% to about 85%.
Claim 11
Dependent Claim
55 words
The process of claim 1 where said curing conditions include a temperature in the range of from about 25° C. to about 300° C., for a time in the range of from about 1 minute to about 600 minutes and at a pressure in the range of from about 14 psi to about 30,000 psi.
Claim 12
Dependent Claim
14 words
The process of claim 1 further characterized in that said cyclosiloxane monomer is 1,3,5,7-tetravinyltetramethylcyclotetrasiloxane.
Claim 13
Dependent Claim
14 words
The process of claim 1 further characterized in that said cyclosiloxane monomer is 1,3,5,7-tetrahydrotetramethylcyclotetrasiloxane.
Claim 14
Dependent Claim
14 words
The process of claim 1 further characterized in that said cyclosiloxane monomer is 1,3,5,7-tetravinyltetrahydrocyclotetrasiloxane.
Claim 15
Dependent Claim
14 words
The process of claim 1 further characterized in that said cyclosiloxane monomer is 1,3,5-trivinyltrimethylcyclotrisiloxane.
Claim 16
Dependent Claim
14 words
The process of claim 1 further characterized in that said cyclosiloxane monomer is 1,3,5-trimethyltrihydrocyclotrisiloxane.
Claim 17
Dependent Claim
48 words
The process of claim 1 further characterized in that said hydrosilylation catalyst is a metal compound where said metal is selected from the group consisting of platinum, cobalt and manganese and is present in an amount ranging from about 1 ppm to about 200 ppm as the metal.
Claim 18
Dependent Claim
8 words
The product of the process of claim 1.
Claim 19
Independent Claim
202 words
A method of forming a high temperature oxidation resistant coating on a carbon-carbon composite comprising the steps: (a) applying a blend of a hydrosilylation catalyst and 1) a cyclosiloxane monomer of formula ##STR4## where n is an integer from 3 to about 20, R is hydrogen, and R' is an alkene having from 2 to about 20 carbon atoms and containing a vinyl-silicon bond, or 2) at least two different cyclosiloxane monomers of the same formula as above and with the same n integer value range where R' is an alkyl group of from 1 to about 20 carbon atoms and in one cyclosiloxane monomer R is hydrogen, and in the others R is an alkene of from 2 to about 20 carbon atoms containing a vinyl-silicon bond to a carbon-carbon composite to afford a coated carbon-carbon composite; (b) curing said coated carbon-carbon composite at curing conditions to produce a cyclosiloxane polymer coated carbon-carbon composite; (c) pyrolyzing said polymer coated carbon-carbon composite under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to produce a black glass coating on said carbon-carbon composite; and (d) recovering said black glass coated carbon-carbon composite.
Claim 20
Independent Claim
202 words
A method of forming a high temperature oxidation resistant coating on a carbon-carbon composite comprising the steps: (a) applying a blend of a hydrosilylation catalyst and 1) a cyclosiloxane monomer of formula ##STR4## where n is an integer from 3 to about 20, R is hydrogen, and R' is an alkene having from 2 to about 20 carbon atoms and containing a vinyl-silicon bond, or 2) at least two different cyclosiloxane monomers of the same formula as above and with the same n integer value range where R' is an alkyl group of from 1 to about 20 carbon atoms and in one cyclosiloxane monomer R is hydrogen, and in the others R is an alkene of from 2 to about 20 carbon atoms containing a vinyl-silicon bond to a carbon-carbon composite to afford a coated carbon-carbon composite; (b) curing said coated carbon-carbon composite at curing conditions to produce a cyclosiloxane polymer coated carbon-carbon composite; (c) pyrolyzing said polymer coated carbon-carbon composite under a non-oxidizing gas atmosphere and at a temperature of about 700° C. to about 1400° C. for a time sufficient to produce a black glass coating on said carbon-carbon composite; and (d) recovering said black glass coated carbon-carbon composite.
Claim 21
Dependent Claim
56 words
The process of claim 18 further characterized in that said curing conditions include a temperature in the range of from about 25° C. to about 300° C., a pressure in the range of from about 14 psi to about 30,000 psi, and a time in the range of from about 1 minute to about 600 minutes.
Claim 22
Dependent Claim
14 words
The process of claim 18 further characterized in that said cyclosiloxane monomer is 1,3,5-trivinyltrimethylcyclotrisiloxane.
Claim 23
Dependent Claim
14 words
The process of claim 18 further characterized in that said cyclosiloxane monomer is 1,3,5,7-tetravinyltetramethylcyclotetrasiloxane.
Claim 24
Dependent Claim
13 words
The process of claim 18 further characterized in that cyclosiloxane monomer is 1,3,5,7-tetrahydrotetramethylcyclotetrasiloxane.
Claim 25
Dependent Claim
14 words
The process of claim 18 further characterized in that said cyclosiloxane monomer is 1,3,5,7-tetravinyltetrahydrocyclotetrasiloxane.
Claim 26
Dependent Claim
48 words
The process of claim 18 further characterized in that said hydrosilylation catalyst is a metal compound where said metal is selected from the group consisting of platinum, cobalt and manganese and is present in an amount ranging from about 1 ppm to about 200 ppm as the metal.
Claim 27
Dependent Claim
8 words
The product of the process of claim 18.
Claim 28
Dependent Claim
69 words
A coated carbon-carbon composite comprising not less than 95% by weight of a carbon-carbon composite which has been coated with a filled black glass where said black glass has the composition SiC x O y in which x ranges from about 0.5 to about 2.0, y ranges from about 0.5 to about 3.0, and where the coating contains from about 15% to about 65% weight percent of a filler.
Claim 29
Dependent Claim
69 words
A coated carbon-carbon composite comprising not less than 95% by weight of a carbon-carbon composite which has been coated with a filled black glass where said black glass has the composition SiC x O y in which x ranges from about 0.5 to about 2.0, y ranges from about 0.5 to about 3.0, and where the coating contains from about 15% to about 65% weight percent of a filler.
Claim 30
Dependent Claim
35 words
The coated composite of claim 26 further characterized in that the filled black glass contains a filler selected from the group consisting of silicon carbide, silicon nitride, titania, hafnia, zirconia, silica, alumina and mixtures thereof.
Claim 31
Dependent Claim
16 words
The coated composite of claim 26 where said filler is a powder, fiber, or a whisker.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1996-07-05 | 1997-01-04 | 1997-07-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-07-05 | 2001-01-04 | 2001-07-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-07-05 | 2005-01-04 | 2005-07-06 | $7700.00 | Window Closed / Lapsed |