Patent US5272240A successfully refreshed from Google Patents.
US5272240A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Fast sol-gel preparation of glasses
Assignee: The University of Texas System
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Filing: 1991-05-29
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Granted: 1993-12-21
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Expires: 2011-05-29
Abstract
Abstract The present invention relates to a method of preparing glasses from metal alkoxides. Glasses are crack-free and prepared rapidly in a single step. Optically clear polysiloxane glasses as thin films may be prepared in a matter of minutes. A glow discharge curing method is disclosed which rapidly cures a wide range of condensation polymers, including polyamide resins and polymethylsiloxane glass films. Fracture-free films up to 100 mu m have been prepared. The glass films may be used as waveguides and to incorporate metals, donor-acceptor molecules and dyes. Stable, crack-free multiple-layered films may be prepared by the disclosed method which can be modified according to desired properties of the glasses.
Inventors
- 👤 Yair Haruvy
- 👤 Stephen E. Webber
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 12:33
CPC Classifications
C; C03; C03C; C03C1/00; C03C1/006; C03C1/008; C09; C09D; C09D4/00
Claims Analysis
Total Claims: 38
Claim 1
Independent Claim
81 words
A rapid method of preparing a stable, optically clear glass, comprising the steps: providing a silicon oxide monomer, said monomer consisting essentially of a monomer having two or three hydrolyzable groups; hydrolyzing the monomer with a near-stoichiometric amount of water; polymerizing the monomer while maintaining a single phase throughout the hydrolyzing and polymerizing wherein hydrolysis and polymerization is accomplished in a total time of less than about 15 minutes; and curing the polymerized monomer to provide a crack-free optically clear glass.
Claim 2
Dependent Claim
81 words
A rapid method of preparing a stable, optically clear glass, comprising the steps: providing a silicon oxide monomer, said monomer consisting essentially of a monomer having two or three hydrolyzable groups; hydrolyzing the monomer with a near-stoichiometric amount of water; polymerizing the monomer while maintaining a single phase throughout the hydrolyzing and polymerizing wherein hydrolysis and polymerization is accomplished in a total time of less than about 15 minutes; and curing the polymerized monomer to provide a crack-free optically clear glass.
Claim 3
Dependent Claim
15 words
The method of claim 1 wherein said hydrolyzing is carried out at an elevated temperature.
Claim 4
Dependent Claim
11 words
The method of claim 1 or 2 further comprising a catalyst.
Claim 5
Dependent Claim
22 words
The method of claim 1, 2, or 3 wherein the metal in the monomer is silicon, titanium, aluminum, barium, copper or yttrium.
Claim 6
Dependent Claim
41 words
The method of claim 4 wherein the monomer has three, four, or five substituents which are independently, an alkoxy group or a nonhydrolyzable group, provided that two or three are alkoxy groups and remaining sites are occupied by a nonhydrolyzable group.
Claim 7
Dependent Claim
10 words
The method of claim 5 wherein the alkoxy is ethoxy.
Claim 8
Dependent Claim
10 words
The method of claim 5 wherein the alkoxy is methoxy.
Claim 9
Dependent Claim
11 words
The method of claim 5 wherein the nonhydrolyzable group is hydrogen.
Claim 10
Dependent Claim
11 words
The method of claim 5 wherein the nonhydrolyzable group is methyl.
Claim 11
Dependent Claim
11 words
The method of claim 5 wherein the nonhydrolyzable group is ethyl.
Claim 12
Dependent Claim
13 words
The method of claim 1 wherein the metal alkoxide monomer is a trialkoxy-substituted.
Claim 13
Dependent Claim
12 words
The method of claim 1 wherein the metal alkoxide monomer is methyltrimethoxy-substituted.
Claim 14
Dependent Claim
12 words
The method of claim 1 wherein the metal alkoxide monomer is dimethyldimethoxy-substituted.
Claim 15
Dependent Claim
15 words
The method of claim 5 wherein the monomer is blocked for hydrolysis at one site.
Claim 16
Dependent Claim
15 words
The method of claim 5 wherein the monomer is blocked for hydrolysis at two sites.
Claim 17
Dependent Claim
19 words
The method of claim 5 wherein the monomer which has five sites is blocked for hydrolysis at three sites.
Claim 18
Dependent Claim
17 words
The method of claim 1 wherein a substantially pure polysiloxane glass is prepared from a trialkoxysilane monomer.
Claim 19
Dependent Claim
11 words
The method of claim 17 wherein the nonhydrolyzable group is hydrogen.
Claim 20
Dependent Claim
12 words
The method of claim 5 wherein the monomer is a substituted silane.
Claim 21
Dependent Claim
10 words
The method of claim 19 wherein the monomer is trimethoxysilane.
Claim 22
Dependent Claim
13 words
The method of claim 1 wherein polymerization is conducted in a nonoxidizing atmosphere.
Claim 23
Dependent Claim
13 words
The method of claim 21 wherein the nonoxidizing atmosphere is nitrogen or argon.
Claim 24
Dependent Claim
18 words
The method of claim 1 wherein the water to monomer molar ratio is between about 0.75 to 1.5.
Claim 25
Dependent Claim
17 words
The method of claim 23 wherein the water to monomer molar ratio is about 0.95 to 1.5.
Claim 26
Dependent Claim
15 words
The method of claim 1 wherein volatile products of the hydrolyzing are removed during polymerization.
Claim 27
Dependent Claim
16 words
The method of claim 25 wherein removal of said products of the hydrolyzing is by distillation.
Claim 28
Dependent Claim
12 words
The method of claim 26 wherein methanol, water or catalyst is removed.
Claim 29
Dependent Claim
15 words
The method of claim 1 wherein said polymerizing is carried out at about 70°-80° C.
Claim 30
Dependent Claim
13 words
The method of claim 1 wherein the polymerized monomer is cured in bulk.
Claim 31
Dependent Claim
35 words
The method of claim 1 further comprising adding a volatile alcohol during polymerization of a monomer having one site occupied by hydrogen, said added alcohol having less volatility than alcohol produced by hydrolyzing said monomer.
Claim 32
Dependent Claim
12 words
The method of claim 1 wherein the glass is cured by air-drying.
Claim 33
Dependent Claim
13 words
The method of claim 1 wherein the glass is cured under inert atmosphere.
Claim 34
Dependent Claim
14 words
The method of claim 3 wherein the catalyst is an acid or base catalyst.
Claim 35
Dependent Claim
11 words
The method of claim 33 wherein the catalyst is hydrochloric acid.
Claim 36
Dependent Claim
10 words
The method of claim 33 wherein the catalyst is dimethylamine.
Claim 37
Dependent Claim
9 words
A glass prepared by the method of claim 1.
Claim 38
Dependent Claim
10 words
A thin film prepared by the method of claim 1.
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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) | 1996-12-20 | 1997-06-21 | 1997-12-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-12-20 | 2001-06-21 | 2001-12-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-12-20 | 2005-06-21 | 2005-12-21 | $7700.00 | Window Closed / Lapsed |