Patent US5206189A successfully refreshed from Google Patents.
US5206189A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Sol-gel method for the preparation of monolithic multicomponent oxide glasses
Assignee: Enichem SpA
•
Filing: 1991-10-25
•
Granted: 1993-04-27
•
Expires: 2011-10-25
Abstract
Abstract An improved method for the production of a monolithic multicomponent oxide glass is achieved by forming an oxide host gel by a sol-gel process, placing the host gel in an aqueous solution of a salt of at least one metal selected from the group consisting of Li, Na, K, Rb, Cs, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Pb, precipitating the metal salt in the gel and sintering the gel containing the precipitated salt. The method can incorporate large amounts of metals into the glass which are otherwise difficult or impossible to incorporate into precursor gels by conventional methods.
Inventors
- 👤 J. Brian Caldwell
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 15:07
CPC Classifications
C; C03; C03C; C03C3/00; C03C3/12; C03C3/14; C03C3/15; C03C3/155; C03C3/04; C03C3/076; C03C3/095; C03C1/00; C03C1/006; C03C3/102; C03C3/105; Y; Y10; Y10S; Y10S501/00; Y10S501/90
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
148 words
A method for the preparation of a monolithic multicomponent oxide glass, comprising the steps of: (a) gelling a mixture comprising a silicon alkoxide, a titanium alkoxide, an alcohol, and an amount of water and acid sufficient to partially hydrolyze the silicon alkoxide, to obtain a gel, wherein said silicon alkoxide is present in an amount sufficient to result in said glass containing from 30 to 98 mole percent of silica; (b) diffusing uniformly into said gel a solution of at least one salt of at least one alkali metal selected from the group consisting of Li, Na, K, Rb, Cs and mixtures thereof in an amount sufficient to result in said glass containing from 5 to 30 mole percent of an oxide of said alkali metal; (c) precipitating said uniformly diffused alkali metal salt in said gel to obtain a gelled mixture; and (d) sintering said gelled mixture.
Claim 2
Independent Claim
148 words
A method for the preparation of a monolithic multicomponent oxide glass, comprising the steps of: (a) gelling a mixture comprising a silicon alkoxide, a titanium alkoxide, an alcohol, and an amount of water and acid sufficient to partially hydrolyze the silicon alkoxide, to obtain a gel, wherein said silicon alkoxide is present in an amount sufficient to result in said glass containing from 30 to 98 mole percent of silica; (b) diffusing uniformly into said gel a solution of at least one salt of at least one alkali metal selected from the group consisting of Li, Na, K, Rb, Cs and mixtures thereof in an amount sufficient to result in said glass containing from 5 to 30 mole percent of an oxide of said alkali metal; (c) precipitating said uniformly diffused alkali metal salt in said gel to obtain a gelled mixture; and (d) sintering said gelled mixture.
Claim 3
Dependent Claim
51 words
The method of claim 1, wherein said solution of said diffusing step further comprises at least one salt of at least one high refractive index modifying metal selected from the group consisting of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Pb.
Claim 4
Dependent Claim
20 words
The method of claim 1, wherein said gelling is conducted at a temperature of from 5° C. to 30° C.
Claim 5
Dependent Claim
27 words
The method of claim 1, further comprising the step of aging said gel at a temperature of from 20° C. to 100° C. before said diffusing step.
Claim 6
Dependent Claim
29 words
The method of claim 1, wherein said diffusing of a solution of said salt into said gel is conducted at a temperature of from 5° C. to 30° C.
Claim 7
Dependent Claim
10 words
The method of claim 5, wherein said solution is aqueous.
Claim 8
Dependent Claim
29 words
The method of claim 1, further comprising the step of drying said gelled mixture at a temperature of from 50° C. to 100° C. prior to said sintering step.
Claim 9
Dependent Claim
20 words
The method of claim 1, wherein said sintering is conducted at a temperature of from 200° C. to 1000° C.
Claim 10
Dependent Claim
24 words
The method of claim 1, wherein said sintering is conducted at a temperature less than the melting point of said monolithic multicomponent oxide glass.
Claim 11
Dependent Claim
42 words
The method of claim 1, wherein in said gelling step said mixture further comprises at least one alkoxide of at least one metal selected from the group consisting of Zr, Hf, Nb, Ta, B, Al, Ga, Ge, Sn, Sb and mixtures thereof.
Claim 12
Dependent Claim
46 words
The method of claim 10, further comprising partially hydrolyzing said silicon alkoxide, then adding said titanium alkoxide and said alkoxide of a metal selected from the group consisting of Zr, Hf, Nb, Ta, B, Al, Ga, Ge, Sn, Sb and mixtures thereof prior to said gelling.
Claim 13
Dependent Claim
18 words
The method of claim 1, wherein in said gelling step said mixture further comprises an alkoxide of aluminum.
Claim 14
Dependent Claim
32 words
The method of claim 1, wherein said gelling is conducted by adding a second portion of water to said mixture to result in a gel sufficiently strong to withstand subsequent processing steps.
Claim 15
Dependent Claim
36 words
The method of claim 1, further comprising the step of aging the gelled mixture for a period of time of from 10 minutes to one week after said gelling step and prior to said diffusing step.
Claim 16
Dependent Claim
28 words
The method of claim 9, wherein said sintering is conducted at a temperature sufficiently high and for a length of time sufficiently long to form a dense glass.
Claim 17
Dependent Claim
43 words
The method of claim 2, wherein said salt of said high refractive index modifying metal is present in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said high refractive index modifying metal.
Claim 18
Dependent Claim
37 words
The method of claim 1, wherein said salt of said alkali metal is present in an amount sufficient to result in said glass containing from 5 to 20 mole percent of an oxide of said alkali metal.
Claim 19
Dependent Claim
33 words
The method of claim 1, wherein said alkoxide of titanium is present in an amount sufficient to result in said glass containing up to 50 mole percent of an oxide of said titanium.
Claim 20
Dependent Claim
34 words
The method of claim 18, wherein said alkoxide of titanium is present in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said titanium.
Claim 21
Dependent Claim
39 words
The method of claim 18, wherein said mixture of said gelling step further comprises an alkoxide of aluminum in an amount sufficient to result in said glass containing up to 30 mole percent of an oxide of said aluminum.
Claim 22
Dependent Claim
34 words
The method of claim 19, wherein said alkoxide of aluminum is present in an amount sufficient to result in said glass containing from 1 to 30 mole percent of an oxide of said aluminum.
Claim 23
Independent Claim
197 words
A method for the preparation of a monolithic multicomponent oxide glass, comprising the steps of: (a) gelling a mixture comprising a silicon alkoxide, an alkoxide of titanium, an alcohol, and an amount of water and acid sufficient to partially hydrolyze the silicon alkoxide, to obtain a gel, wherein said silicon alkoxide is present in an amount sufficient to result in said glass containing from 30 to 98 mole percent of silica, and said alkoxide of titanium is present in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said titanium; (b) diffusing uniformly into said gel a solution of at least one salt of at least one high refractive index modifying metal selected from the group consisting of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Pb and mixtures thereof in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said high refractive index modifying metal; (c) precipitating said high refractive index modifying metal salt in said gel to obtain a gelled mixture; and (d) sintering said gelled mixture.
Claim 24
Independent Claim
197 words
A method for the preparation of a monolithic multicomponent oxide glass, comprising the steps of: (a) gelling a mixture comprising a silicon alkoxide, an alkoxide of titanium, an alcohol, and an amount of water and acid sufficient to partially hydrolyze the silicon alkoxide, to obtain a gel, wherein said silicon alkoxide is present in an amount sufficient to result in said glass containing from 30 to 98 mole percent of silica, and said alkoxide of titanium is present in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said titanium; (b) diffusing uniformly into said gel a solution of at least one salt of at least one high refractive index modifying metal selected from the group consisting of Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Pb and mixtures thereof in an amount sufficient to result in said glass containing from 1 to 40 mole percent of an oxide of said high refractive index modifying metal; (c) precipitating said high refractive index modifying metal salt in said gel to obtain a gelled mixture; and (d) sintering said gelled mixture.
Claim 25
Dependent Claim
61 words
The method of claim 22, wherein said solution of said diffusing step further comprises at least one salt of at least one alkali metal selected from the group consisting of Li, Na, K, Rb, Cs and mixtures thereof in an amount sufficient to result in said glass containing from 5 to 30 mole percent of an oxide of said alkali metal.
Claim 26
Dependent Claim
39 words
The method of claim 22, wherein said mixture of said gelling step further comprises an alkoxide of aluminum in a amount sufficient to result in said glass containing up to 30 mole percent of an oxide of said aluminum.
Claim 27
Dependent Claim
33 words
The method of claim 22, further comprising an alkoxide of aluminum present in an amount sufficient to result in said glass containing from 1 to 30 percent of an oxide of said aluminum.
Claim 28
Dependent Claim
18 words
The method of claim 22, wherein said high refractive index modifying metal in said diffusing step is lead.
Claim 29
Dependent Claim
18 words
The method of claim 23, wherein said high refractive index modifying metal in said diffusing step is lead.
References Cited (Backward Citations)
US4278632A
Cited
US4397666A
Cited
US4686195A
Cited
US4801399A
Cited
US4816072A
Cited
US4767433A
Cited
US4797376A
Cited
US4902650A
Cited
US5069700A
Cited
US5068208A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1996-04-26 | 1996-10-26 | 1997-04-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 2000-04-26 | 2000-10-26 | 2001-04-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2004-04-26 | 2004-10-26 | 2005-04-27 | $7700.00 | Window Closed / Lapsed |