Patent US1471468A successfully refreshed from Google Patents.
US4801318A
Expired / Lapsed
US
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Silica glass formation process
Assignee: Seiko Epson Corp
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Filing: 1987-01-29
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Granted: 1989-01-31
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Expires: 2007-01-29
Abstract
Abstract In a forming a silica glass at low temperature, a fumed silica is added to a hydrolyzed solution of a metal alcoxide. 0.2-5 mol of fumed silica is added to 1 mol of metal alcoxide. Being uniformly dispersed, the solution is gelled and dried to be dry gel and then sintered to be non-porous. This process allows a practically large sized silica glass to be materialized which has been impossible by the previous sol-gel technology. In addition, a further large silica glass can be prepared by adjusting pH value to 3-6 with addition of base in the sol solution.
Inventors
- 👤 Motoyuki Toki
- 👤 Sadao Kanbe
- 👤 Satoru Miyashita
- 👤 Tetsuhiko Takeuchi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 06:50
CPC Classifications
C; C03; C03C; C03C1/00; C03C1/006; C03B; C03B19/00; C03B19/12; C03C3/00; C03C3/04; C03C3/06; C03C2201/00; C03C2201/02; C03C2203/00; C03C2203/20; C03C2203/26; C03C2203/34; Y; Y02; Y02P; Y02P40/00; Y02P40/50; Y02P40/57; Y10; Y10S; Y10S65/00; Y10S65/901
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
95 words
A process for forming a monolithic silica glass article, comprising: hydrolyzing a silicon alkoxide in solution to form a hydrolyzed solution; adding an effective amount of fumed silica for preventing cracking during the process, which would provide cracks in the glass article, to the hydrolyzed solution to form a sol solution; gelling the sol solution to form a gel; drying the gel to form a dry gel; and sintering the dry gel at a temperature effective to form a glass thereby to form a large monolithic silica glass article without said cracking during the process.
Claim 2
Dependent Claim
95 words
A process for forming a monolithic silica glass article, comprising: hydrolyzing a silicon alkoxide in solution to form a hydrolyzed solution; adding an effective amount of fumed silica for preventing cracking during the process, which would provide cracks in the glass article, to the hydrolyzed solution to form a sol solution; gelling the sol solution to form a gel; drying the gel to form a dry gel; and sintering the dry gel at a temperature effective to form a glass thereby to form a large monolithic silica glass article without said cracking during the process.
Claim 3
Dependent Claim
19 words
The process of claim 1, wherein the fumed silica is formed by hydrolyzing SiCl 4 with an oxy-hydrogen flame.
Claim 4
Dependent Claim
16 words
The process of claim 1, wherein said fumed silica is derived from a sodium silicate solution.
Claim 5
Dependent Claim
18 words
The process of claim 1, wherein said fumed silica is obtained by hydrolyzing a silicon alkoxide with ammonia.
Claim 6
Dependent Claim
22 words
The process of claim 1, further including the step of uniformly dispersing the fumed silica in the sol solution by ultrasonic vibration.
Claim 7
Dependent Claim
28 words
The process of claim 1, further including the step of dispersing the fumed silica in the sol solution by centrifugal separation to insure uniform dispersion of fumed silica.
Claim 8
Dependent Claim
12 words
The process of claim 1, wherein the silicon alkoxide is silicon ethoxide.
Claim 9
Dependent Claim
17 words
The process of claim 1, wherein the hydrolyzed silicon alkoxide is silicon ethoxide hydrolyzed with hydrochloric acid.
Claim 10
Dependent Claim
27 words
The process of claim 1, including the step of adjusting the pH of the sol solution to between about 3 and 6 by addition of a base.
Claim 11
Dependent Claim
25 words
The process of claim 1, wherein the pH of the sol solution is adjusted to between about 4 and 4.5 by addition of a base.
Claim 12
Dependent Claim
17 words
The process of claim 9, wherein the base is any one of ammonia and an organic base.
Claim 13
Dependent Claim
23 words
The process of claim 11, wherein the ammonia is selected from the group consisting of ammonia water, ammonia gas and an ammonia solution.
Claim 14
Dependent Claim
33 words
The process of claim 11, wherein the organic base is selected from the group of triethylamine, an aqueous solution of triethylamine, pyridine, an aqueous solution of pyridine, aniline or an aqueous aniline solution.
Claim 15
Dependent Claim
50 words
The process of claim 1, further including the step of drying the sol solution to a gel, and drying the gel to a dry gel in a mold having a lid covering the mold, said lid formed with aperatures comprising less than 50% of the surface area of the lid.
Claim 16
Dependent Claim
36 words
The process of claim 9, wherein the sol solution is gelled in a mold having a lid covering the mold and formed with openings comprising less than about 20% of the surface area of the lid.
Claim 17
Dependent Claim
37 words
The process of claim 1, wherein the gel is formed at temperatures between about 5° and 60° C. and the gel is dried to a dry gel at a drying temperature between about 20° and 120° C.
Claim 18
Dependent Claim
24 words
The process of claim 16, wherein the gel is heated to the drying temperature at a rate less than about 120° C. per hour.
Claim 19
Dependent Claim
30 words
The process of claim 1, wherein the sintering of the dry gel includes the steps of (a) removing absorbed water; (b) removing carbon and (c) making the dry gel non-porous.
Claim 20
Dependent Claim
56 words
The process of claim 18, including at least one heating step of removing absorbed water by heating the dry gel to a first selected temperature between about 20° and 400° C. at a heating rate of less than 400° C. per hour and maintaining the dried gel at the selected temperature for at least one hour.
Claim 21
Dependent Claim
59 words
The process of claim 19, including at least one heating step of removing carbon by heating the dry gel to a second selected temperature between about 400° and 1200° C. at a heating rate of between about 30° to 400° C. per hour and maintaining the second selected temperature for a period of more than at least 3 hours.
Claim 22
Dependent Claim
46 words
The process of claim 20, including at least one heating step of making the dry gel non-porous by heating the dry gel to a third selected temperature between about 1000° and 1400° C. at a heating rate of between about 30° and 400° C. per hour.
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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) | 1992-01-31 | 1992-08-01 | 1993-01-31 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-01-31 | 1996-08-01 | 1997-01-31 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-01-31 | 2000-08-01 | 2001-01-31 | $7700.00 | Window Closed / Lapsed |