US4622056A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of preparing silica glass
Assignee: Seiko Epson Corp
•
Filing: 1986-02-06
•
Granted: 1986-11-11
•
Expires: 2006-02-06
Abstract
Abstract A method for preparing high quality silica glass articles is provided. The glass is prepared by hydrolyzing silicon alkoxide with a basic reagent to yield a first solution, hydrolyzing a silicon alkoxide with an acid reagent to yield a second solution, mixing the first solution with the second solution at a predetermined mixing rate to yield a sol solution, pouring the sol solution into a container, gelling the sol solution to a wet gel, drying the wet gel to a dry gel, and sintering the dry gel to yield a silica glass.
Inventors
- 👤 Nobutaka Matsuo
- 👤 Yoshitaka Itoh
- 👤 Sadao Kanbe
- 👤 Haruo Osafune
- 👤 Masanobu Motoki
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 22:25
CPC Classifications
C; C03; C03B; C03B37/00; C03B37/01; C03B37/012; C03B37/014; C03B37/016; C03B19/00; C03B19/12; C03C; C03C1/00; C03C1/006; Y; Y02; Y02P; Y02P40/00; Y02P40/50; Y02P40/57
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
85 words
A method for preparing silica glass articles, comprising: preparing a first solution by hydrolyzing silicon alkoxide with a basic reagent; preparing a second solution by hydrolyzing silicon alkoxide with an acid reagent; mixing the first and second solutions together at a predetermined mixing ratio in order to yield a sol solution; pouring the sol solution into a container; gelling the sol solution to a wet gel; drying the wet gel to a dry gel; and sintering the dry gel to yield a silica glass article.
Claim 2
Independent Claim
85 words
A method for preparing silica glass articles, comprising: preparing a first solution by hydrolyzing silicon alkoxide with a basic reagent; preparing a second solution by hydrolyzing silicon alkoxide with an acid reagent; mixing the first and second solutions together at a predetermined mixing ratio in order to yield a sol solution; pouring the sol solution into a container; gelling the sol solution to a wet gel; drying the wet gel to a dry gel; and sintering the dry gel to yield a silica glass article.
Claim 3
Dependent Claim
19 words
The method of claim 1, wherein the sintering step comprises closing pores in the dry gel under He atmosphere.
Claim 4
Dependent Claim
19 words
The method of claim 1, wherein the sintering step comprises closing pores in the dry gel under reduced pressure.
Claim 5
Dependent Claim
27 words
The method of claim 1, wherein the sintering step comprises closing pores in the dry gel under reduced pressure after processing the dry gel in He atmosphere.
Claim 6
Dependent Claim
23 words
The method of claim 2, wherein hydroxyl groups and chlorine and fluorine are eliminated from the dry gel prior to closing the pores.
Claim 7
Dependent Claim
23 words
The method of claim 3, wherein hydroxyl groups and chlorine and fluorine are eliminated from the dry gel prior to closing the pores.
Claim 8
Dependent Claim
23 words
The method of claim 4, wherein hydroxyl groups and chlorine and fluorine are eliminated from the dry gel prior to closing the pores.
Claim 9
Dependent Claim
13 words
The method of claim 1, wherein the silica glass article is a plate.
Claim 10
Dependent Claim
12 words
The method of claim 1, wherein the silica glass article is cylindrical.
Claim 11
Dependent Claim
12 words
The method of claim 1, wherein the silica glass article is tubular.
Claim 12
Independent Claim
132 words
A method for preparing silica glass articles comprising: preparing a first solution by hydrolyzing silicon alkoxide with a basic reagent; preparing a second solution by hydrolyzing silicon alkoxide with an acid reagent; mixing the first and second solutions together at a predetermined mixing ratio in order to yield a sol solution; pouring the sol solution into a container; gelling the sol solution to a wet gel; drying the wet gel to a dry gel; and sintering the dry gel by a method comprising the steps of: removing absorbed water; removing carbon; accelerating the dehydration condensation reaction; closing pores in the dry gel under He atmosphere or under reduced pressure or under reduced pressure after processing the dry gel in He atmosphere; and vitrifying the dry gel to yield a silica glass article.
Claim 13
Independent Claim
132 words
A method for preparing silica glass articles comprising: preparing a first solution by hydrolyzing silicon alkoxide with a basic reagent; preparing a second solution by hydrolyzing silicon alkoxide with an acid reagent; mixing the first and second solutions together at a predetermined mixing ratio in order to yield a sol solution; pouring the sol solution into a container; gelling the sol solution to a wet gel; drying the wet gel to a dry gel; and sintering the dry gel by a method comprising the steps of: removing absorbed water; removing carbon; accelerating the dehydration condensation reaction; closing pores in the dry gel under He atmosphere or under reduced pressure or under reduced pressure after processing the dry gel in He atmosphere; and vitrifying the dry gel to yield a silica glass article.
Claim 14
Dependent Claim
26 words
The method of claim 11, wherein the mean particle diameter of the fine particle silica in the first solution is between about 0.01 and 1.0 microns.
Claim 15
Dependent Claim
22 words
The method of claim 11, wherein the concentration of fine particle silica in the first solution is greater than about 0.05 g/ml.
Claim 16
Dependent Claim
26 words
The method of claim 11, wherein the mixing ratio of the first and second solutions is between about 0 and 100 and about 100 and 0.
Claim 17
Dependent Claim
26 words
The method of claim 14, wherein the mixing ratio of the first and second solutions is between about 20 and 85 and about 80 and 15.
Claim 18
Dependent Claim
21 words
The method of claim 11, wherein the effective concentration of silica in the sol solution is greater than about 0.10 g/ml.
Claim 19
Dependent Claim
23 words
The method of claim 11, wherein the pH of the sol solution is adjusted to a value greater than 3 prior to gelling.
Claim 20
Dependent Claim
40 words
The method of claim 11, wherein the sol solution is placed in a container having a predetermined shape prior to gelling and is maintained at a temperature between about 10° and 50° C. until the gel shrinks to some degree.
Claim 21
Dependent Claim
29 words
The method of claim 11, wherein the wet gel is dried in a container having openings amounting to less than about 10% of the surface area of the container.
Claim 22
Dependent Claim
18 words
The method of claim 11, wherein the inner surface of the container is formed of a hydrophobic material.
Claim 23
Dependent Claim
35 words
The method of claim 11, wherein the wet gel is dried by heating the gel to a temperature between about 50° and 160° C. at a heating rate of less than 120° C. per hour.
Claim 24
Dependent Claim
55 words
The method of claim 11, wherein absorbed water is removed by heating the dry gel to a first selected temperature in the range between about 20° and 400° C. at a heating rate of less than about 400° C. per hour and maintaining the gel at the first selected temperature for at least one hour.
Claim 25
Dependent Claim
39 words
The method of claim 11, wherein carbon is removed by heating the gel to a second selected temperature in the range between about 400° and 900° C. at a heating rate between about 30° and 400° C. per hour.
Claim 26
Dependent Claim
53 words
The method of claim 11, wherein the dehydration condensation reaction is accelerated by heating the gel to a third selected temperature between about 900° and 1300° C. at a heating rate between about 1° and 400° C. per hour and maintaining the gel at the third selected temperature for at least 30 minutes.
Claim 27
Dependent Claim
56 words
The method of claim 11, wherein pores are closed in the gel by heating the gel to a fourth selected temperature in the range between about 900° and 1400° C. at a heating rate between about 30° and 400° C. per hour and maintaining the gel at the fourth selected temperature for at least one hour.
Claim 28
Dependent Claim
35 words
The method of claim 11, wherein the dry gel is vitrified by heating the gel to a fifth selected temperature and maintaining the gel at the fifth selected temperature for a predetermined period of time.
Claim 29
Dependent Claim
27 words
The method of claim 11, wherein the sintering process further comprises removing hydroxyl groups and chlorine and fluorine prior to closing the pores in the dry gel.
Claim 30
Dependent Claim
42 words
The method of claim 11, wherein the materials used to prepare the first and second solutions are of high purity and microrefuse and foreign particles are eliminated by distillation or filtration with a filter having a mesh of less than 0.2 microns.
Claim 31
Dependent Claim
27 words
The method of claim 11, wherein the steps before pouring the sol solution into a container are performed in a clean environment of less than class 3000.
Claim 32
Dependent Claim
27 words
The method of claim 29, wherein the steps before pouring the sol solution into a container are performed in a clean environment of less than class 100.
Claim 33
Dependent Claim
38 words
The method of claim 11, wherein the first solution is subjected to centrifugal force between about 50 and 10,000 G and the supernatant solution is mixed with the second solution prior to mixing the first and second solutions.
Claim 34
Dependent Claim
35 words
The method of claim 11, wherein at least one of the first solution, the second solution and the sol solution is filtered at least once using a filter having a mesh finer than 50 microns.
Claim 35
Dependent Claim
22 words
The method of claim 11, wherein the sol solution is processed under reduced pressure at least once prior to the gelation step.
Claim 36
Dependent Claim
23 words
The method of claim 11, wherein the sol solution is gelled with the application of centrifugal force between about 50 and 500 G.
References Cited (Backward Citations)
JPS55167143A
Cited
US4317668A
Cited
US4389233A
Cited
US4426216A
Cited
JPS59102833A
Cited
JPS6027615A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-11-10 | 1990-05-12 | 1990-11-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-11-10 | 1994-05-12 | 1994-11-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-11-10 | 1998-05-12 | 1998-11-11 | $7700.00 | Window Closed / Lapsed |