US3791808A
Expired / Lapsed
US
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Method for producing glass ceramics
Assignee: OI Glass Inc
•
Filing: 1971-12-23
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Granted: 1974-02-12
•
Expires: 1991-12-23
Abstract
Abstract There is disclosed a process for the preparation of glass ceramics from a thermally crytallizable oxide product which is formed by hydrolysis and condensation reactions and wherein the oxide product is produced and is converted to a glass ceramic at temperatures below the normal liquidus or normal melting temperature of an oxide composition corresponding to the oxide composition of the oxide product.
Inventors
- 👤 I Thomas
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 18:07
CPC Classifications
C; C03; C03C; C03C10/00; C03C1/00; C03C1/006; Y; Y10; Y10S; Y10S516/00; Y10S516/924; Y10S516/928; Y10S65/00; Y10S65/901
Claims Analysis
Total Claims: 27
Claim 1
Independent Claim
22 words
reacting the partially hydrolyzed product with a metal alkoxide so as to form a clear solution of a soluble, further hydrolyzable metallosiloxane,
Claim 2
Dependent Claim
20 words
The process of claim 1 wherein said oxide product is of a composition corresponding to a thermally crystallizable lithia-aluminosilicate composition.
Claim 3
Dependent Claim
28 words
reacting said clear solution of a soluble, partially hydrolyzed silicon alkoxide with a metal alkoxide so as to form a clear solution of a soluble, further hydrolyzable metallosiloxane,
Claim 4
Dependent Claim
24 words
reacting the partially hydrolyzed product of step 1 with a metal alkoxide so as to form a solution of a soluble, further hydrolyzable metallosiloxane,
Claim 5
Dependent Claim
37 words
reacting said further hydrolyzable metallosiloxane with an additional quantity of water, said additional quantity of water being sufficient to hydrolyze residual alkoxy groups in the metallosiloxane so as to form a solution which converts to a gel,
Claim 6
Dependent Claim
45 words
reacting said clear solution of a soluble, further hydrolyzable metallosiloxane with an additional quantiTy of water, said additional quantity of water being sufficient to hydrolyze said further hydrolyzable metallosiloxane so as to form a solution which converts to a gel structure containing a cross-linked metallosiloxane,
Claim 7
Dependent Claim
23 words
The process of claim 2 wherein lithia, alumina and silica are present in mole ratios of between about 1:1:2 to about 1:1:15 respectively.
Claim 8
Dependent Claim
32 words
reacting said further hydrolyzable metallosiloxane with a quantity of water sufficient to hydrolyze residual alkoxy groups in the metallosiloxane so as to form a clear solution which subsequently converts to a gel,
Claim 9
Dependent Claim
61 words
converting said gel to a particulate oxide product, (B) heating said body to a temperature and for a time sufficient to thermally crystallize said thermally crystallizable oxide product to a glass-ceramic, said oxide product being formed at and said process being performed at temperatures below the normal melting temperature of an oxide composition corresponding to the composition of said oxide product.
Claim 10
Dependent Claim
14 words
The process of claim 3 wherein said ratios are about 1:1:3 to about 1:1:8.
Claim 11
Dependent Claim
3 words
drying the gel,
Claim 12
Dependent Claim
53 words
heating said gel so as to form an oxide product, consolidating said oxide product to a unitary body, said oxide product and said unitary body being formed at and said thermal crystallization being performed at temperatures below the normal melting temperature of an oxide composition corresponding to the composition of said oxide product.
Claim 13
Dependent Claim
21 words
crushing the dried gel so as to produce a particulate mass having a particle size of less than about 0.2 microns,
Claim 14
Dependent Claim
34 words
The process of claim 1 wherein said oxide product is a composition corresponding to a thermally crystallizable magnesia-aluminosilicate, wherein magnesia, alumina and silica are present in mole ratios of about 1:1:2.5 to about 1:1:4.
Claim 15
Dependent Claim
43 words
The process of claim 1 wherein n is 0 and wherein said hydrolysis is effected with about 0.3 to about 1.5 equivalents of water per equivalent of said silicon alkoxide and wherein said hydrolysis is effected in the presence of an organic solvent.
Claim 16
Dependent Claim
79 words
heating said particulate mass to a temperature of about 300* C. to about 500* C. for at least about 1 hour so as to remove residual organic components therefrom and form said oxide product, B. heating said body to a temperature and for a time sufficient to thermally crystallize said thermally crystallizable precursor to a glass-ceramic, said process being performed at temperatures below the normal melting temperature of an oxide composition corresponding to the composition of said oxide product.
Claim 17
Dependent Claim
22 words
A process which comprises: (A) consolidating particles of a thermally crystallizable oxide product into a unitary body, said product being prepared by:
Claim 18
Dependent Claim
42 words
The process of claim 5 wherein step 2 comprises drying said gel, crushing the dried gel to a particle size of less than about 0.2 microns and heating said crushed and dried gel to a temperature sufficient to remove residual organic components.
Claim 19
Dependent Claim
67 words
The process of claim 7 wherein n is 0 and wherein said hydrolysis is effected with about 0.3 to about 1.5 equivalents of water per equivalent of said silicon alkoxide and wherein said hydrolysis is effected in the presence of an organic solvent and wherein at least part of the water reacted in step 3 is a water solution of a metal salt of an organic acid.
Claim 20
Dependent Claim
39 words
The process of claim 9 wherein said silicon alkoxide is ethyl silicate and wherein about 1 equivalent of water per about 1 equivalent of silicon alkoxide is used to effect hydrolysis and wherein said catalyst is a mineral acid.
Claim 21
Dependent Claim
15 words
The process of claim 10 wherein said solvent is ethanol and said acid is HCl.
Claim 22
Dependent Claim
35 words
The process of claim 9 wherein said oxide product is of a composition corresponding to a thermally crystallizable lithia-alumina-silicate, wherein lithia, alumina and silica are present in molar proportions of about 1:1:3 to about 1:1:8.
Claim 23
Dependent Claim
36 words
A process for forming a glass-ceramic comprising: A. consolidating particles having a size less than about 0.2 microns of a thermally crystallizable, oxide product into a unitary body, said product being prepared by steps which comprise:
Claim 24
Dependent Claim
38 words
The process of claim 13 wherein at least part of said additional water which is reacted in Step 3 is a water solution of a metal salt of an organic acid which is convertible to a metal oxide.
Claim 25
Dependent Claim
49 words
The process of claim 14 wherein n is 0 and wherein the amount of water which is combined with said silicon alkoxide is about 0.3 to about 1.5 equivalent per equivalent of silicon alkoxide and where said combining is done in the presence of a C1 to C3 alcohol.
Claim 26
Dependent Claim
24 words
A process for forming a glass ceramic which comprises thermally crystallizing a consolidated unitary thermally crystallizable body, said thermally crystallizable body being prepared by:
Claim 27
Dependent Claim
48 words
The method of claim 16 wherein said silicon alkoxide is silicon tetraethoxide and wherein at least part of said additional quantity of water is a water solution of a metal salt which is decomposable to a metal oxide and further wherein said hydrolysis catalyst is a mineral acid.
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) | 1977-02-11 | 1977-08-13 | 1978-02-12 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-02-11 | 1981-08-13 | 1982-02-12 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-02-11 | 1985-08-13 | 1986-02-12 | $7700.00 | Window Closed / Lapsed |