Patent US5116637A successfully refreshed from Google Patents.
US5116637A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Amine catalysts for the low temperature conversion of silica precursors to silica
Assignee: Dow Silicones Corp
•
Filing: 1990-06-04
•
Granted: 1992-05-26
•
Expires: 2010-06-04
Abstract
Abstract This invention relates to a low temperature method of converting coatings of hydrogen silsesquioxane resin or hydrolyzed or partially hydrolyzed R X Si(OR) 4-X to ceramic silica coatings. The method comprises applying a silica precursor coating to a substrate, exposing the coating to an environment comprising an amine and subjecting the coating to a temperature sufficient to yield the ceramic coating. The methods of the invention are particularly applicable to applying coatings on electronic devices.
Inventors
- 👤 Ronald H. Baney
- 👤 Carl J. Bilgrien
- 👤 Dennis W. Broderick
- 👤 II Leslie E. Carpenter
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 12:26
CPC Classifications
C; C09; C09D; C09D143/00; C09D143/04; C04; C04B; C04B41/00; C04B41/45; C04B41/50; C04B41/5025; C04B41/5035; C04B2111/00; C04B2111/00474; C04B2111/00844
Claims Analysis
Total Claims: 26
Claim 1
Independent Claim
75 words
A method of forming a ceramic coating on an electronic device comprising: coating said device with a solution comprising a solvent and hydrogen silsesquioxane resin; evaporating said solvent to deposit a hydrogen silsesquioxane resin coating on said device; exposing said coating to an environment comprising an amine and moisture to catalyze the conversion of the coating; and subjecting the catalyzed coating to a temperature sufficient to facilitate conversion of said coating to a ceramic coating.
Claim 2
Independent Claim
75 words
A method of forming a ceramic coating on an electronic device comprising: coating said device with a solution comprising a solvent and hydrogen silsesquioxane resin; evaporating said solvent to deposit a hydrogen silsesquioxane resin coating on said device; exposing said coating to an environment comprising an amine and moisture to catalyze the conversion of the coating; and subjecting the catalyzed coating to a temperature sufficient to facilitate conversion of said coating to a ceramic coating.
Claim 3
Dependent Claim
50 words
The method of claim 1 wherein the solvent is selected from the group consisting of alcohols, aromatic hydrocarbons, alkanes, ketones, esters, glycol ethers or cyclic dimethylsiloxanes and wherein said solvent is present in an amount sufficient to dissolve the hydrogen silsesquioxane to between about 0.1 and about 50 weight percent.
Claim 4
Dependent Claim
27 words
The method of claim 2 wherein the catalyzed coating is subjected to a temperature of about 20° to about 400° C. for up to about 6 hours.
Claim 5
Dependent Claim
78 words
The method of claim 3 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 final ceramic coating contains 0.1 to 30 percent by weight modifying ceramic oxide.
Claim 6
Dependent Claim
35 words
The method of claim 3 wherein the solution also contains a platinum or rhodium catalyst in an amount of about 15 to about 500 ppm platinum or rhodium based on the weight of hydrogen silsesquioxane.
Claim 7
Dependent Claim
35 words
The method of claim 4 wherein the solution also contains a platinum or rhodium catalyst in an amount of about 15 to about 500 ppm platinum or rhodium based on the weight of hydrogen silsesquioxane.
Claim 8
Dependent Claim
27 words
The method of claim 3 wherein the coating is exposed to an environment comprising a liquid amine and moisture and the method of exposure is by immersion.
Claim 9
Dependent Claim
35 words
The method of claim 7 wherein the coating is exposed to the liquid amine for up to about 6 hours at a temperature of between about 20° C. and the boiling point of the amine.
Claim 10
Dependent Claim
17 words
The method of claim 8 wherein the exposure is for about 1-3 hours at about 20°-200° C.
Claim 11
Dependent Claim
29 words
The method of claim 9 wherein the catalyzed coating is subjected to a temperature of between about 20° and about 200° C. for between about 0.5 and 6 hours.
Claim 12
Dependent Claim
32 words
The method of claim 3 wherein the coating is exposed to amine vapors and moisture for up to about 6 hours at a temperature of between about 20° C. and 400° C.
Claim 13
Dependent Claim
20 words
The method of claim 11 wherein the exposure is for about 1-3 hours at about 20° to about 200° C.
Claim 14
Dependent Claim
29 words
The method of claim 12 wherein the catalyzed coating is subjected to a temperature of between about 20° and about 200° C. for between about 0.5 and 6 hours.
Claim 15
Independent Claim
117 words
A method of forming a ceramic coating on an electronic device comprising: coating said device with a solution comprising a solvent and hydrolyzed or partially hydrolyzed R x Si(OR) 4-x , wherein 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 of hydrolyzed or partially hydrolyzed R x Si(OR) 4-x on said device; exposing said preceramic coating to an environment comprising an amine and moisture to catalyze the conversion of the preceramic coating, provided the amine is not an alkanol amine; and subjecting the catalyzed preceramic coating to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 16
Independent Claim
117 words
A method of forming a ceramic coating on an electronic device comprising: coating said device with a solution comprising a solvent and hydrolyzed or partially hydrolyzed R x Si(OR) 4-x , wherein 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 of hydrolyzed or partially hydrolyzed R x Si(OR) 4-x on said device; exposing said preceramic coating to an environment comprising an amine and moisture to catalyze the conversion of the preceramic coating, provided the amine is not an alkanol amine; and subjecting the catalyzed preceramic coating to a temperature sufficient to facilitate conversion of said preceramic coating to a ceramic coating.
Claim 17
Dependent Claim
56 words
The method of claim 14 wherein the solvent is selected from the group consisting of alcohols, aromatic hydrocarbons, alkanes, ketones, esters, glycol ethers or cyclic dimethylsiloxanes and wherein the solvent 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 18
Dependent Claim
28 words
The method of claim 15 wherein the catalyzed preceramic coating is subjected to a temperature of about 20° to about 400° C. for up to about 6 hours.
Claim 19
Dependent Claim
78 words
The method of claim 16 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 final ceramic coating contains 0.1 to 30 percent by weight modifying ceramic oxide.
Claim 20
Dependent Claim
26 words
The method of claim 16 wherein the preceramic coating is exposed to an environment comprising a liquid amine and the method of exposure is by immersion.
Claim 21
Dependent Claim
36 words
The method of claim 18 wherein the preceramic coating is exposed to the liquid amine for up to about 6 hours at a temperature of between about 20° C. and the boiling point of the amine.
Claim 22
Dependent Claim
17 words
The method of claim 19 wherein the exposure is for about 1-3 hours at about 20°-200° C.
Claim 23
Dependent Claim
30 words
The method of claim 20 wherein the catalyzed preceramic coating is subjected to a temperature of between about 20° and about 200° C. for between about 0.5 and 6 hours.
Claim 24
Dependent Claim
31 words
The method of claim 16 wherein the preceramic coating is exposed to amine vapors for up to about 6 hours at a temperature of between about 20° C. and 400° C.
Claim 25
Dependent Claim
20 words
The method of claim 22 wherein the exposure is for about 1-3 hours at about 20° to about 200° C.
Claim 26
Dependent Claim
30 words
The method of claim 23 wherein the catalyzed preceramic coating is subjected to a temperature of between about 20° and about 200° C. for between about 0.5 and 6 hours.
References Cited (Backward Citations)
US3923705A
Cited
US4384013A
Cited
JPS57118592A
Cited
US4636440A
Cited
JPS62265129A
Cited
US4756977A
Cited
US4749631A
Cited
US4911992A
Cited
US4749631B1
Cited
US4900582A
Cited
US4847162A
Cited
US4842888A
Cited
US5059448A
Cited
US5063267A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1995-05-26 | 1995-11-25 | 1996-05-26 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1999-05-26 | 1999-11-25 | 2000-05-26 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2003-05-26 | 2003-11-25 | 2004-05-26 | $7700.00 | Window Closed / Lapsed |