US5262201A
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US
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Low temperature process for converting silica precursor coatings to ceramic silica coatings by exposure to ammonium hydroxide or an environment to which water vapor and ammonia vapor have been added
Assignee: Dow Silicones Corp
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Filing: 1990-06-04
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Granted: 1993-11-16
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Expires: 2010-06-04
Abstract
Abstract This invention relates to a method of forming a ceramic coating on a substrate. The method comprises coating the substrate with a solution comprising a solvent and a silica precursor followed by evaporating the solvent to form a preceramic coating. The preceramic coating is then exposed to an environment comprising ammonium hydroxide or an environment to which water vapor and ammonia vapor have been added to facilitate conversion of the silica precursor to the ceramic coating. The preceramic coating is then subjected to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Inventors
- 👤 Grish Chandra
- 👤 Loren A. Haluska
- 👤 Keith W. Michael
- 👤 Carl J. Bilgrien
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 23:21
CPC Classifications
C; C09; C09D; C09D183/00; C09D183/02; H; H10; H10P; H10P14/00; H10P14/60; H10P14/69; H10P14/6903; C04; C04B; C04B41/00; C04B41/009; C04B41/45; C04B41/50; C04B41/5025; C04B41/5035; C04B41/80; C04B41/81; C04B41/85; C04B41/87; H10P14/65; H10P14/6516; H10P14/6529; H10P14/66; H10P14/668; H10P14/6681; H10P14/6684; H10P14/6686; C04B2111/00; C04B2111/00474; C04B2111/00844; H10P14/63; H10P14/6326; H10P14/6342
Claims Analysis
Total Claims: 37
Claim 1
Independent Claim
78 words
A method of forming a ceramic coating on a substrate comprising: coating said substrate with a solution comprising a solvent and hydrogen silsesquioxane resin; evaporating said solvent to deposit a preceramic coating on said substrate; exposing said preceramic coating to an environment comprising ammonium hydroxide or an environment into which water vapor and ammonia vapor have been introduced; and subjecting the preceramic coating to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 2
Independent Claim
78 words
A method of forming a ceramic coating on a substrate comprising: coating said substrate with a solution comprising a solvent and hydrogen silsesquioxane resin; evaporating said solvent to deposit a preceramic coating on said substrate; exposing said preceramic coating to an environment comprising ammonium hydroxide or an environment into which water vapor and ammonia vapor have been introduced; and subjecting the preceramic coating to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 3
Dependent Claim
99 words
The method of claim 1 wherein the hydrogen silsesquioxane resin is selected from the group consisting of (HSiO 3/2 ) n , a polymer having units of the formula HSi(OH) a O 3-x/2 and a polymer having units of the formula HSi(OH) x (OR) y O z/2 , wherein each R is independently an organic group which, when bonded to silicon through the oxygen atom, forms a hydrolyzable substituent, a=0-2, x=0-2, y=0-2, z=1-3, x+y+z=3, n is an integer greater than 3 and the average value of y over all of the units of the polymer is greater than 0.
Claim 4
Dependent Claim
45 words
The method of claim 2 wherein the solvent is selected from the group consisting of alcohols, aromatic hydrocarbons, alkanes, ketones, esters or glycol ethers and is present in an amount sufficient to dissolve the hydrogen silsesquioxane to between about 0.1 and about 50 weight percent.
Claim 5
Dependent Claim
27 words
The method of claim 3 wherein the preceramic coating is subjected to a temperature of about 20° to about 500° C. for up to about 6 hours.
Claim 6
Dependent Claim
28 words
The method of claim 4 wherein the preceramic coating is subjected to a temperature of about 20° to about 500° C. for between about 0.5 about 6 hours.
Claim 7
Dependent Claim
77 words
The method of claim 4 wherein the solution also contains a modifying ceramic oxide precursor comprising a compound containing an element selected from the group consisting of titanium, zirconium, aluminum, tantalum, vanadium, niobium, boron and phosphorous wherein the compound contains at least one hydrolyzable substituent selected from the group consisting of alkoxy or acyloxy and the compound is present in an amount such that the ceramic coating contains 0.1 to 30 percent by weight modifying ceramic oxide.
Claim 8
Dependent Claim
33 words
The method of claim 4 wherein the solution also contains a platinum or rhodium catalyst in an amount of about 5 to about 500 ppm platinum based on the weight of hydrogen silsesquioxane.
Claim 9
Dependent Claim
33 words
The method of claim 6 wherein the solution also contains a platinum or rhodium catalyst in an amount of about 5 to about 500 ppm platinum based on the weight of hydrogen silsesquioxane.
Claim 10
Dependent Claim
37 words
The method of claim 4 wherein the preceramic coating is exposed to an environment comprising a concentrated ammonium hydroxide solution and the method of exposure is by immersing the preceramic coating in said concentrated ammonium hydroxide solution.
Claim 11
Dependent Claim
21 words
The method of claim 9 wherein the preceramic coating is exposed to the ammonium hydroxide for up to about 4 hours.
Claim 12
Dependent Claim
17 words
The method of claim 10 wherein the exposure is for about 1-3 hours at about room temperature.
Claim 13
Dependent Claim
28 words
The method of claim 11 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 0.5 and 2 hours.
Claim 14
Dependent Claim
43 words
The method of claim 4 wherein the preceramic coating is exposed to an environment into which water vapor and ammonia vapor have been introduced for up to about 4 hours at a temperature of between about 20 ° C. and about 500° C.
Claim 15
Dependent Claim
22 words
The method of claim 13 wherein the exposure is for about 1 to 3 hours at about 20° to about 200° C.
Claim 16
Dependent Claim
26 words
The method of claim 14 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 1-2 hours.
Claim 17
Dependent Claim
42 words
The method of claim 4 wherein the preceramic coating is sequentially exposed to both concentrated ammonium hydroxide for up to about 4 hours and an environment into which water vapor and ammonia vapor have been introduced for up to about 4 hours.
Claim 18
Dependent Claim
26 words
The method of claim 16 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 1-2 hours.
Claim 19
Dependent Claim
48 words
The method of claim 1 wherein the preceramic coating is simultaneously exposed to an environment comprising ammonium hydroxide and an environment into which water vapor and ammonia vapor have been introduced and subjected to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 20
Dependent Claim
18 words
The method of claim 4 wherein the preceramic coating is subjected to said temperature under an ammonia environment.
Claim 21
Independent Claim
104 words
A method of forming a ceramic coating on a substrate comprising: coating said substrate with a solution comprising a solvent and hydrolyzed or partially hydrolyzed R x Si(OR) 4-x , in which R is an aliphatic, alicyclic or aromatic substituent of 1-20 carbon atoms and x is 0-2; evaporating said solvent to deposit a preceramic coating on said substrate; exposing said preceramic coating to an environment comprising ammonium hydroxide or an environment into which water vapor and ammonia vapor have been introduced; and subjecting the preceramic coating to a temperature above room temperature to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 22
Independent Claim
104 words
A method of forming a ceramic coating on a substrate comprising: coating said substrate with a solution comprising a solvent and hydrolyzed or partially hydrolyzed R x Si(OR) 4-x , in which R is an aliphatic, alicyclic or aromatic substituent of 1-20 carbon atoms and x is 0-2; evaporating said solvent to deposit a preceramic coating on said substrate; exposing said preceramic coating to an environment comprising ammonium hydroxide or an environment into which water vapor and ammonia vapor have been introduced; and subjecting the preceramic coating to a temperature above room temperature to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 23
Dependent Claim
51 words
The method of claim 20 wherein the solvent is selected from the group consisting of alcohols, aromatic hydrocarbons, alkanes, ketones, esters or glycol ethers and is present in an amount sufficient to dissolve the hydrolyzed or partially hydrolyzed R x Si(OR) 4-x to between about 0.1 and about 50 weight percent.
Claim 24
Dependent Claim
27 words
The method of claim 21 wherein the preceramic coating is subjected to a temperature of about 20° to about 500° C. for up to about 6 hours.
Claim 25
Dependent Claim
28 words
The method of claim 22 wherein the preceramic coating is subjected to a temperature of about 20° to about 500° C. for between about 0.5 about 6 hours.
Claim 26
Dependent Claim
77 words
The method of claim 23 wherein the solution also contains a modifying ceramic oxide precursor comprising a compound containing an element selected from the group consisting of titanium, zirconium, aluminum, tantalum, vanadium, niobium, boron and phosphorous wherein the compound contains at least one hydrolyzable substituent selected from the group consisting of alkoxy or acyloxy and the compound is present in an amount such that the ceramic coating contains 0.1 to 30 percent by weight modifying ceramic oxide.
Claim 27
Dependent Claim
37 words
The method of claim 22 wherein the preceramic coating is exposed to an environment comprising a concentrated ammonium hydroxide solution and the method of exposure is by immersing the preceramic coating in said concentrated ammonium hydroxide solution.
Claim 28
Dependent Claim
21 words
The method of claim 25 wherein the preceramic coating is exposed to the ammonium hydroxide for up to about 4 hours.
Claim 29
Dependent Claim
17 words
The method of claim 26 wherein the exposure is for about 1-3 hours at about room temperature.
Claim 30
Dependent Claim
28 words
The method of claim 27 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 0.5 and 2 hours.
Claim 31
Dependent Claim
42 words
The method of claim 22 wherein the preceramic coating is exposed to an environment into which water vapor and ammonia vapor have been introduced for up to about 4 hours at a temperature of between about 20° C. and about 500° C.
Claim 32
Dependent Claim
22 words
The method of claim 29 wherein the exposure is for about 1 to 3 hours at about 20° to about 200° C.
Claim 33
Dependent Claim
26 words
The method of claim 30 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 1-2 hours.
Claim 34
Dependent Claim
42 words
The method of claim 22 wherein the preceramic coating is sequentially exposed to both concentrated ammonium hydroxide for up to about 4 hours and an environment into which water vapor and ammonia vapor have been introduced for up to about 4 hours.
Claim 35
Dependent Claim
26 words
The method of claim 32 wherein the preceramic coating is subjected to a temperature between about 20° and about 200° C. for between about 1-2 hours.
Claim 36
Dependent Claim
50 words
The method of claim 20 wherein the preceramic coating is simultaneously exposed to an environment comprising ammonium hydroxide and an environment into which water vapor and ammonia vapor have been introduced and subjected to a temperature above room temperature to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 37
Dependent Claim
18 words
The method of claim 22 wherein the preceramic coating is subjected to said temperature under an ammonia environment.
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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) | 1996-11-15 | 1997-05-17 | 1997-11-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-11-15 | 2001-05-17 | 2001-11-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-11-15 | 2005-05-17 | 2005-11-16 | $7700.00 | Window Closed / Lapsed |