US4806328A
Expired / Lapsed
US
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Method of manufacturing monolithic glass members
Assignee: US Philips Corp
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Filing: 1985-09-30
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Granted: 1989-02-21
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Expires: 2005-09-30
Abstract
Abstract Monolithic glass members are prepared by first hydrolyzing a solution of tetraethoxysilane in alcohol with an acid medium, and then gelating in a basic medium while using acid and base mediums to form compounds that volatilize during drying and sintering the gel. Substances, if any, which in the form of oxides can form a glass with SiO 2 , are added after hydrolyzing and prior to gelation.
Inventors
- 👤 Joseph G. Van Lierop
- 👤 Arnoldus B. M. Bogemann
- 👤 Willy J. B. Felder
- 👤 Albert Huizing
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 21:43
CPC Classifications
C; C01; C01B; C01B33/00; C01B33/113; C01B33/12; C01B33/14; C01B33/157; C01B33/158; C01B33/1585; C03; C03B; C03B19/00; C03B19/12; C03B37/00; C03B37/01; C03B37/012; C03B37/014; C03B37/016; C03C; C03C1/00; C03C1/006
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
155 words
A method of manufacturing monolithic glass members comprising the steps of preparing a monolithic gel by dissolving tetraethoxysilane (C 2 H 5 O) 4 Si) in an ethanol, hydrolyzing said tetraethoxysilane in said ethanol by adding water and an acid to form a hydrolyzed solution, adding water and a base material to said hydrolyzed solution, said base material being added in a quantity to neutralize said acid, forming a neutralized compound from said acid and said base material, said neutralized compound being sufficiently volatile to subsequently escape, drying said gel by placing said gel into a hermetically sealed container under a pre-pressure of a gas, wherein said pre-pressure is at least 50 bars, heating said gel to a temperature above the critical temperature of said gel, said pre-pressure being sufficiently high to prevent boiling of the solvent of said gel at said temperature, and then densifying said gel by said heating and removing said pre-pressure.
Claim 2
Independent Claim
155 words
A method of manufacturing monolithic glass members comprising the steps of preparing a monolithic gel by dissolving tetraethoxysilane (C 2 H 5 O) 4 Si) in an ethanol, hydrolyzing said tetraethoxysilane in said ethanol by adding water and an acid to form a hydrolyzed solution, adding water and a base material to said hydrolyzed solution, said base material being added in a quantity to neutralize said acid, forming a neutralized compound from said acid and said base material, said neutralized compound being sufficiently volatile to subsequently escape, drying said gel by placing said gel into a hermetically sealed container under a pre-pressure of a gas, wherein said pre-pressure is at least 50 bars, heating said gel to a temperature above the critical temperature of said gel, said pre-pressure being sufficiently high to prevent boiling of the solvent of said gel at said temperature, and then densifying said gel by said heating and removing said pre-pressure.
Claim 3
Dependent Claim
23 words
A method according to claim 1, wherein said gas is selected from the group consisting of hydrogen, helium, nitrogen, oxygen, chlorine, and argon.
Claim 4
Dependent Claim
12 words
A method according to claim 1, wherein said gas is thionyl chloride.
Claim 5
Dependent Claim
22 words
A method according to claim 1, wherein said step of heating is carried out at a temperature between 275 and 325° C.
Claim 6
Dependent Claim
28 words
A method according to claim 1, wherein at least one compound which forms a glass with SiO 2 is added to said hydrolyzed solution prior to gelation occurring.
Claim 7
Dependent Claim
34 words
A method according to claim 1, wherein a fluorine compound selected from the group consisting of HF, NH 4 F and NH 4 F--HF is added to said hydrolyzed solution prior to gelation occurring.
Claim 8
Dependent Claim
33 words
A method according to claim 1, wherein a compound selected from the group consisting of aluminum, titanium, boron, germanium, and a rare earth is added to said hydrolyzed solution prior to gelation occurring.
Claim 9
Dependent Claim
42 words
A method according to claim 1, wherein a compound selected from the group consisting of aluminum, titanium, boron, germanium and a rare earth is added to said hydrolyzed solution prior to gelation occurring, said compound decomposing at temperatures used to form oxides.
Claim 10
Dependent Claim
21 words
A method according to claim 1, wherein said acid is selected from the group consisting of HCl and HNO 3 .
Claim 11
Dependent Claim
25 words
A method according to claim 9, wherein said base material is selected from the group consisting of NH 4 OH and an organic nitrogen base.
Claim 12
Dependent Claim
14 words
A method according to claim 1, wherein said pre-pressure is at least 80 bars.
Claim 13
Dependent Claim
15 words
A method according to claim 1 or claim 4, wherein said temperature is 300° C.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1992-02-21 | 1992-08-22 | 1993-02-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-02-21 | 1996-08-22 | 1997-02-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-02-21 | 2000-08-22 | 2001-02-21 | $7700.00 | Window Closed / Lapsed |