US3811918A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for producing protective glass coatings
Assignee: OI Glass Inc
•
Filing: 1971-12-20
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Granted: 1974-05-21
•
Expires: 1991-12-20
Abstract
Abstract A process for providing a silicate glass coated and protected inorganic substrate which comprises applying a substantially gel resistant, mineral acid stabilized, clear solution having a pH of less than about 1.5 of a substrate compatible glass composition in the form of a glass precursor onto the substrate and then heating the precursor to a temperature and for a time sufficient to convert the precursor into a silicate glass coating on the substrate. The precursor is prepared by hydrolyzing prescribed silicon alkoxides with less than a stoichiometric amount of water so as to prepare a clear solution of a partially hydrolyzed silicon alkoxide, which partially hydrolyzed silicon alkoxide solution is then reacted with an aqueous solution of a metal oxide forming compound so as to form a solution of the precursor or with a metal alkoxide so as to form a clear solution of a further hydrolyzable metallosiloxane, which latter clear solution of the further hydrolyzable metallosiloxane is then reacted with either a quantity of water sufficient to hydrolyze residual alkoxy groups or with an aqueous solution of a metal compound which is convertible to a metal oxide so as to form a solution of the glass precursor.
Inventors
- 👤 L Levene
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 01:32
CPC Classifications
C; C04; C04B; C04B41/00; C04B41/009; C03; C03C; C03C17/00; C03C17/02; C04B41/45; C04B41/50; C04B41/5022; C04B41/80; C04B41/81; C04B41/85; C04B41/86; C07; C07F; C07F7/00; C07F7/02; C07F7/04; Y; Y10; Y10S; Y10S65/00; Y10S65/901
Claims Analysis
Total Claims: 35
Claim 1
Independent Claim
104 words
combining said solution of a partially hydrolyzed silicon alkoxide with a metal alkoxide of the formula M(OR'')X, wherein M represents a metal, R'' is an alkyl of 1 to 6 carbon atoms, and X is an integer equal to the valence of M, or of the formula M1M2(OR)X, wherein M1 and M2 are metals, R is an alkyl of 1 to 6 carbon atoms and X is an integer equal to the combined valences of M1 and M2 and allowing said combined ingredients to react so as to form a clear solution of a soluble, further hydrolyzable metallosiloxane having residual OR and OR'' groups,
Claim 2
Dependent Claim
104 words
combining said solution of a partially hydrolyzed silicon alkoxide with a metal alkoxide of the formula M(OR'')x wherein M represents a metal, R'' is an alkyl of 1 to 6 carbon atoms, and x is an integer equal to the valence of M, or a compound of the formula M1M2 (OR)x, wherein M1 and M2 are metals, R is an alkyl of 1 to 6 carbon atoms, and x is an integer equal to the combined valences of M1 and M2, and allowing said combined ingredients to react so as to form a clear solution of a soluble, further-hydrolyzable metallosiloxane having residual alkoxy groups,
Claim 3
Dependent Claim
29 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, and
Claim 4
Dependent Claim
60 words
reacting said partially hydrolyzed silicon alkoxide with an aqueous solution of a metal compound which is convertible to a metal oxide below about 600*C. so as to form a clear solution of said glass precursor; II. heating said glass precursor to a temperature and for a time sufficient to convert same to a silicate glass coating on said inorganic substrate.
Claim 5
Dependent Claim
23 words
reacting the partially hydrolyzed silicon alkoxide with a metal alkoxide so as to form a clear solution of a soluble, further hydrolyzable metallosiloxane;
Claim 6
Dependent Claim
41 words
The process of claim 1 wherein the silicon alkoxide is hydrolyzed with at least about 0.3 equivalent of water per equivalent of silicon alkoxide and wherein said metal compound is a metal salt of an organic acid or of nitric acid.
Claim 7
Dependent Claim
23 words
reacting the partially hydrolyzed silicon alkoxide with a metal alkoxide so as to form a clear solution of a soluble, further hydrolyzable metallosiloxane;
Claim 8
Dependent Claim
64 words
reacting said clear solution of a soluble, further hydrolyzable metallosiloxane with an aqueous solution of a metal compound which is convertible to a metal oxide below about 600*C. so as to form a clear solution of said glass precursor; II. heating said glass precursor to a temperature and for a time sufficient to convert same to a silicate glass coating on the inorganic substrate.
Claim 9
Dependent Claim
60 words
reacting said clear solution of a soluble, further hydrolyzable metallosiloxane with an additional quantity of water sufficient to hydrolyze residual alkoxy groups in the metallosiloxane so as to form a clear solution of said precursor; II. heating said glass precursor to a temperature and for a time sufficient to convert same to a silicate glass coating on the inorganic substrate.
Claim 10
Dependent Claim
60 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 clear solution, II. heating said precursor to a temperature and for a time sufficient to convert same to a silicate glass coating on said inorganic substrate.
Claim 11
Dependent Claim
87 words
reacting said solution of a soluble metallosiloxane with an additional quantity of water, said additional quantity of water being sufficient to react with said residual alkoxy groups so as to obtain a clear solution, and wherein at least part of said additional water is a water solution of a metal salt which decomposes to an oxide below about 600* C., II. heating said deposit of said glass precursor to a temperature and for a time sufficient to convert same to a silicate glass coating on said substrate.
Claim 12
Dependent Claim
43 words
reacting said solution of a soluble metallosiloxane with a water solution of a metal compound which is convertible to a metal oxide, sufficient water being employed to react with said residual OR groups and OR'' groups so as to obtain a clear solution,
Claim 13
Dependent Claim
46 words
The process of claim 2 wherein n in said silicon alkoxide is O and wherein the hydrolysis is effected with about 0.3 to about 1.5 equivalents of water per equivalent of silicon alkoxide, and wherein said hydrolysis is done in the presence of an organic solvent.
Claim 14
Dependent Claim
81 words
adjusting the pH of said latter solution to between about 0.5 to 1, wherein said elevated temperature and the rate of said spraying are so selected so that essentially no wetting of said alumina takes place and so that the solvent substantially evaporates upon contact with said alumina, leaving a deposit thereon of said glass precursor and II. heating said precursor to a temperature and for a time sufficient to convert same to a smooth silicate glass coating on the alumina.
Claim 15
Dependent Claim
11 words
The process of claim 3 wherein the silicon alkoxide is tetraethylsilicate.
Claim 16
Dependent Claim
12 words
The process of claim 3 wherein said substrate is an alumina substrate.
Claim 17
Dependent Claim
40 words
The process of claim 5 wherein said applying is done by spraying said substrate while at an elevated temperature, said temperature and the spraying rate being so selected so as to essentially prevent wetting of the surface of said substrate.
Claim 18
Dependent Claim
37 words
The process of claim 3 wherein said applied solution contains said glass precursor in a concentration of about 5 to about 20 percent by weight based on the total weight of said precursor''s theoretical oxide glass composition.
Claim 19
Dependent Claim
36 words
The process of claim 7 wherein said glass composition consists essentially of, on a theoretical oxide basis, about 37 percent SiO2, about 10 percent Al2O3, about 35 percent BaO, and about 18 percent B2O3 by weight.
Claim 20
Dependent Claim
44 words
The process of claim 1 and further including adjusting the pH of the clear solution of said glass precursor, as formed after said reaction with said aqueous solution of a metal compound, with a mineral acid to a pH of less than about 1.5.
Claim 21
Dependent Claim
12 words
The process of claim 9 wherein said mineral acid is nitric acid.
Claim 22
Dependent Claim
53 words
A process for providing a silicate glass coated and protected inorganic substrate which comprises: I. applying a substantially gel resistant, mineral acid stabilized clear solution, having a pH of less than about 1.5, of a substrate-compatible glass composition in the form of a glass precursor onto said substrate, said soLution being prepared by:
Claim 23
Dependent Claim
19 words
The process of claim 11 wherein said applied solution has a pH of between about 1.5 and about 1.
Claim 24
Dependent Claim
44 words
The process of claim 11 wherein the pH of the solution of said glass precursor after reaction with said additional quantity of water is between about 2.5 and about 5 and further including the step of adjusting said pH to less than about 1.5.
Claim 25
Dependent Claim
53 words
A process for providing a silicate glass coated and protected inorganic substrate which comprises: I. applying a substantially gel resistant, mineral acid stabilized clear solution, having a pH of less than about 1.5, of a substrate-compatible glass composition in the form of a glass precursor onto said substrate, said solution being prepared by:
Claim 26
Dependent Claim
17 words
The process of claim 14 wherein said metal compound is a metal salt of an organic acid.
Claim 27
Dependent Claim
40 words
A process for providing a silicate glass coated and protected inorganic substrate which comprises: I. applying a clear solution having a pH of less than about 1.5 of a hydrolyzed glass precursor onto said substrate, said precursor being prepared by:
Claim 28
Dependent Claim
31 words
The process of claim 16 wherein at least part of said additional quantity of water is a water solution of a metal compound which decomposes to an oxide below about 600*C.
Claim 29
Dependent Claim
42 words
The process of claim 17 wherein said metal alkoxide is a compound of the formula M(OR'')X wherein M represents a metal, R'' represents an alkyl of 1 to 6 carbon atoms, and X is an integer equal to the valence of M.
Claim 30
Dependent Claim
45 words
The process of claim 17 wherein said metal alkoxide is a double metal alkoxide of the formula M1M2(OR)X wherein M1 and M2 are metals, R is an alkyl of 1 to 7 carbon atoms and X corresponds to the combined valences of M1 and M2.
Claim 31
Dependent Claim
102 words
The process of claim 16 wherein n is O, the amount of water which is combined with said silicon alkoxide is about one equivalent per equivalent of silicon alkoxide, said combining being done in the presence of a C1 to C6 alcohol, and wherein said acid hydrolysis catalyst is present in an amount sufficient to provide a pH of between about 2.5 to about 5 and further including the step of adjusting the pH of the clear solution formed by said reacting of said clear solution of said further hydrolyzable metallosiloxane with an additional quantity of water to less than about 1.5.
Claim 32
Dependent Claim
43 words
A process for increasing the smoothness of the surface of an alumina substrate which comprises: I. spraying a clear solution in a solvent of an alumina-compatible, hydrolyzed silicate-glass precursor onto said alumina substrate while at an elevated temperature, said precursor being prepared by
Claim 33
Dependent Claim
28 words
The process of claim 21 wherein said precursor is heated to form said silicate glass coating within a period of time of about 15 to about 90 seconds.
Claim 34
Dependent Claim
30 words
The process of claim 22 wherein said silicon alkoxide and water is reacted in the presence of ethanol and wherein said elevated temperature is between about 150*C. to about 300*C.
Claim 35
Dependent Claim
85 words
A process for providing a silicate glass-coated and protected inorganic substrate which comprises: I. spraying a clear solution in a solvent of a hydrolyzed silicate glass precursor onto said substrate while said substrate is at an elevated temperature, said temperature and the spraying rate being so selected so as to essentially prevent wetting of the surface of said substrate and so that the solvent substantially evaporates upon contact with said substrate, leaving a deposit thereon of said silicate glass precursor, said precursor being prepared by
References Cited (Backward Citations)
No citation records indexed.
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-05-20 | 1977-11-19 | 1978-05-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-05-20 | 1981-11-19 | 1982-05-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-05-20 | 1985-11-19 | 1986-05-21 | $7700.00 | Window Closed / Lapsed |