US4397666A
Expired / Lapsed
US
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Method of producing glass from metal alkoxide solution
Assignee: Central Glass Co Ltd
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Filing: 1981-10-27
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Granted: 1983-08-09
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Expires: 2001-10-27
Abstract
Abstract In producing silica glass, which may contain additional metal(s) such as Ti or Zr, from a solution of a silicon alkoxide, mixed with alkoxide(s) of the additional metal(s) where necessary, in water and a hydrophilic organic solvent by shaping the solution into a desired form such as a coating film on a substrate, self-supporting film, fiber or lump when the solution exhibits a suitably high viscosity and sufficiently heating the shaped solution, a water-soluble organic polymeric substance is added to the solution as a viscosity adjusting agent to soon increase the viscosity of the solution to the desirable level. Therefore, shaping of the solution can be performed without awaiting the progress of hydrolysis of the alkoxide in the solution, and the glass can be obtained with improved uniformity of its properties. A cellulose ether is preferred as the viscosity adjusting agent, and hydroxypropyl cellulose is particularly preferable.
Inventors
- 👤 Michiharu Mishima
- 👤 Yuji Yamamoto
- 👤 Kensuke Makita
- 👤 Sumio Sakka
- 👤 Kanichi Kamiya
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 15:05
CPC Classifications
C; C04; C04B; C04B41/00; C04B41/009; C03; C03B; C03B19/00; C03B19/12; C03B37/00; C03B37/01; C03B37/011; C03C; C03C1/00; C03C1/006; C03C1/008; C03C3/00; C03C3/04; C03C3/06; C04B41/45; C04B41/50; C04B41/5022; C04B41/80; C04B41/81; C04B41/85; C04B41/86; C03C2201/00; C03C2201/02; C03C2201/06; C03C2201/30; C03C2201/40; C03C2201/42; C03C2203/00; C03C2203/20; C03C2203/26; C03C2203/30; Y; Y02; Y02P; Y02P40/00; Y02P40/50; Y02P40/57; Y10; Y10S; Y10S65/00; Y10S65/901
Claims Analysis
Total Claims: 21
Claim 1
Independent Claim
190 words
In a method of producing glass from a solution comprising a silicon alkoxide, water and a hydrophilic organic solvent, wherein the silicon alkoxide in the solution undergoes hydrolysis so that the viscosity of the solution gradually increases; the method comprising the steps of shaping the material of said solution into a desired form when said solution exhibits an appropriate viscosity for shaping wherein the gelled shaped solution material undergoes gelation, and heating the gelled shaped solution to a temperature sufficient to convert the shaped solution into a glass of the desired form; the improvement comprising the step of adding a water-soluble cellulose ether selected from the group consisting of hydroxypropyl cellulose, hydroxyethyl cellulose, hydroxypropylmethyl cellulose, methyl cellulose and ethyl cellulose to said solution as a viscosity increasing agent in an amount effective to increase the viscosity of the solution to from 5 to 30 centipoises at room temperature, the increase in viscosity being effected substantially independently of the progress of said hydrolysis, wherein the shaping of the solution is performed when the viscosity reaches the viscosity for shaping without awaiting the progress of said hydrolysis to effect a shaping viscosity.
Claim 2
Dependent Claim
190 words
In a method of producing glass from a solution comprising a silicon alkoxide, water and a hydrophilic organic solvent, wherein the silicon alkoxide in the solution undergoes hydrolysis so that the viscosity of the solution gradually increases; the method comprising the steps of shaping the material of said solution into a desired form when said solution exhibits an appropriate viscosity for shaping wherein the gelled shaped solution material undergoes gelation, and heating the gelled shaped solution to a temperature sufficient to convert the shaped solution into a glass of the desired form; the improvement comprising the step of adding a water-soluble cellulose ether selected from the group consisting of hydroxypropyl cellulose, hydroxyethyl cellulose, hydroxypropylmethyl cellulose, methyl cellulose and ethyl cellulose to said solution as a viscosity increasing agent in an amount effective to increase the viscosity of the solution to from 5 to 30 centipoises at room temperature, the increase in viscosity being effected substantially independently of the progress of said hydrolysis, wherein the shaping of the solution is performed when the viscosity reaches the viscosity for shaping without awaiting the progress of said hydrolysis to effect a shaping viscosity.
Claim 3
Dependent Claim
23 words
A method according to claim 1, wherein said cellulose ether is added to said solution in the form of solution in an alcohol.
Claim 4
Dependent Claim
28 words
A method according to claim 1, wherein said silicon alkoxide is a sole alkoxide contained in said solution so that said glass is a practically pure silica glass.
Claim 5
Dependent Claim
23 words
A method according to claim 3, wherein said solution further comprises an acid which serves as a catalyst for hydrolysis of said alkoxide.
Claim 6
Dependent Claim
23 words
A method according to claim 4, wherein said acid is selected from the group consisting of nitric acid, hydrochloric acid and acetic acid.
Claim 7
Dependent Claim
42 words
A method according to claim 1, wherein said solution further comprises at least one additional metal alkoxide other than silicon alkoxide so that said glass is a modified silica glass containing in the glass matrix at least one metal other than silicon.
Claim 8
Dependent Claim
24 words
A method according to claim 3 or 6, wherein said silicon alkoxide is selected from the group consisting of silicon methoxide and silicon ethoxide.
Claim 9
Dependent Claim
23 words
A method according to claim 6, wherein said additional metal alkoxide is selected from the group consisting of titanium tetraisopropoxide and zirconium propoxide.
Claim 10
Dependent Claim
31 words
A method according to claim 3 or 6, wherein the mole ratio of said water to the total metal alkoxide in said solution is in the range from 1:1 to 20:1.
Claim 11
Dependent Claim
14 words
A method according to claim 9, wherein said organic solvent is a lower alcohol.
Claim 12
Dependent Claim
30 words
A method according to claim 10, wherein the mole ratio of said organic solvent to the total metal alkoxide in said solution is in the range from 3:1 to 10:1.
Claim 13
Dependent Claim
46 words
A method according to claim 1, wherein the step of shaping said solution into a desired form is accomplished by coating a surface of a solid body with said solution so that said glass is produced in the form of a coating film on said surface.
Claim 14
Dependent Claim
32 words
A method according to claim 12, wherein the amount of said viscosity adjusting agent is such that said appropriate viscosity is in the range from 7 to 25 centipoises at room temperature.
Claim 15
Dependent Claim
34 words
A method according to claim 12, wherein the coating of said surface with said solution is accomplished by immersing said solid body into said solution and withdrawing the wetted solid body from said solution.
Claim 16
Dependent Claim
14 words
A method according to claim 12, wherein said solid body is a glass body.
Claim 17
Dependent Claim
14 words
A method according to claim 12, wherein said solid body is a ceramic body.
Claim 18
Dependent Claim
24 words
A method according to claim 12, wherein the coating of said surface with said solution is accomplished by applying said solution to said surface.
Claim 19
Dependent Claim
22 words
A method according to claim 12, wherein the thickness of said coating film is in the range from 0.3 to 1.0 microns.
Claim 20
Dependent Claim
24 words
A method according to claim 1 or 12, wherein said cellulose ether is added to said solution at the stage of preparing said solution.
Claim 21
Dependent Claim
21 words
A method according to claim 1, wherein said solution contains a water-soluble salt of a transition element as a coloring agent.
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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) | 1986-08-08 | 1987-02-07 | 1987-08-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1990-08-08 | 1991-02-07 | 1991-08-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1994-08-08 | 1995-02-07 | 1995-08-09 | $7700.00 | Window Closed / Lapsed |