Patent US5084206A successfully refreshed from Google Patents.
US5084206A
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Doped crystalline compositions and a method for preparation thereof
Assignee: EIDP Inc
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Filing: 1990-02-02
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Granted: 1992-01-28
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Expires: 2010-02-02
Abstract
Abstract A composition is disclosed which consists essentially of doped crystalline MTiOXO 4 (wherein M is selected from the group consisting of K, Rb and Tl, X is selected from the group consisting of P and As) which contain at least about 100 ppm total of at least one dopant selected from the group consisting of Ga, Al and Si. The compositions generally have low ionic conductivity, and may be prepared using an improved flux process wherein Ga, Al and/or Si dopant is added to the flux in a total amount of at least about 0.5 mole % and the crystallization temperature is controlled to provide a crystalline composition containing the desired amount of dopant.
Inventors
- 👤 Albert A. Ballman
- 👤 John D. Bierlein
- 👤 August Ferretti
- 👤 Thurman E. Gier
- 👤 Patricia A. Morris
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 19:07
CPC Classifications
C; C30; C30B; C30B29/00; C30B29/10; C30B29/16; C30B29/22; C30B29/14; C30B9/00
Claims Analysis
Total Claims: 49
Claim 1
Independent Claim
86 words
A composition consisting essentially of doped crystalline MTiOXO 4 wherein M is selected from the group consisting of K, Rb and Tl, and X is selected from the group consisting of P and As, said MTiOXO 4 being crystallized from a flux and containing at least one dopant selected from the group consisting of Ga, Al and Si in an amount, totaling at least about 100 ppm, effective to reduce the ionic conductivity of the doped crystalline composition compared to a crystalline composition without said dopant.
Claim 2
Dependent Claim
86 words
A composition consisting essentially of doped crystalline MTiOXO 4 wherein M is selected from the group consisting of K, Rb and Tl, and X is selected from the group consisting of P and As, said MTiOXO 4 being crystallized from a flux and containing at least one dopant selected from the group consisting of Ga, Al and Si in an amount, totaling at least about 100 ppm, effective to reduce the ionic conductivity of the doped crystalline composition compared to a crystalline composition without said dopant.
Claim 3
Dependent Claim
17 words
The composition of claim 1 containing at least about 200 ppm of said at least one dopant.
Claim 4
Dependent Claim
15 words
The composition of claim 2 wherein said doped crystalline MTiOXO 4 is a single crystal.
Claim 5
Dependent Claim
10 words
The composition of claim 3 wherein the dopant is Ga.
Claim 6
Dependent Claim
10 words
The composition of claim 3 wherein the dopant is Al.
Claim 7
Dependent Claim
10 words
The composition of claim 3 wherein the dopant is Si.
Claim 8
Dependent Claim
16 words
The composition of claim 3 in which the dopant is a mixture of Ga and Si.
Claim 9
Dependent Claim
9 words
The composition of claim 3 wherein X is P.
Claim 10
Dependent Claim
9 words
The composition of claim 3 wherein X is As.
Claim 11
Dependent Claim
9 words
The composition of claim 3 wherein M is K.
Claim 12
Dependent Claim
9 words
The composition of claim 10 wherein X is P.
Claim 13
Dependent Claim
10 words
The composition of claim 11 wherein the dopant is Ga.
Claim 14
Dependent Claim
10 words
The composition of claim 11 wherein the dopant is Al.
Claim 15
Dependent Claim
10 words
The composition of claim 11 wherein the dopant is Si.
Claim 16
Dependent Claim
15 words
The composition of claim 11 wherein the dopant is a mixture of Ga and Si.
Claim 17
Dependent Claim
9 words
The composition of claim 10 wherein X is As.
Claim 18
Dependent Claim
10 words
The composition of claim 16 wherein the dopant is Ga.
Claim 19
Dependent Claim
198 words
In a process for producing a single crystal of MTiOXO 4 , wherein M is selected from the group consisting of K, Rb, and Tl, X is selected from the group consisting of P and As, comprising the steps of preparing a substantially isothermal melt containing the components for forming MTiOXO 4 crystals and a flux comprising oxides of M and X; suspending a seed crystal of MTiOXO 4 in the melt; slowly decreasing the temperature of the melt; and continuing decreasing the temperature until crystallization of the crystalline composition is completed; an improvement for reducing the ionic conductivity of the single crystal comprising adding to the flux at least about 0.5 mole percent total of at least one dopant selected from the group consisting of Ga, Al and Si, calculated as the oxide and based upon the total moles of MTiOXO 4 crystals formable from the components in the melt; and controlling the crystallizing temperature to provide a doped single crystal of MTiOXO 4 which contains said dopant in an amount, totaling at least about 100 ppm, effective to reduce the ionic conductivity of the single crystal compared to a single crystal prepared without adding said dopant.
Claim 20
Dependent Claim
198 words
In a process for producing a single crystal of MTiOXO 4 , wherein M is selected from the group consisting of K, Rb, and Tl, X is selected from the group consisting of P and As, comprising the steps of preparing a substantially isothermal melt containing the components for forming MTiOXO 4 crystals and a flux comprising oxides of M and X; suspending a seed crystal of MTiOXO 4 in the melt; slowly decreasing the temperature of the melt; and continuing decreasing the temperature until crystallization of the crystalline composition is completed; an improvement for reducing the ionic conductivity of the single crystal comprising adding to the flux at least about 0.5 mole percent total of at least one dopant selected from the group consisting of Ga, Al and Si, calculated as the oxide and based upon the total moles of MTiOXO 4 crystals formable from the components in the melt; and controlling the crystallizing temperature to provide a doped single crystal of MTiOXO 4 which contains said dopant in an amount, totaling at least about 100 ppm, effective to reduce the ionic conductivity of the single crystal compared to a single crystal prepared without adding said dopant.
Claim 21
Dependent Claim
39 words
The improved process of claim 18 wherein the temperature of the melt when the seed crystal is suspended therein is within the range of from about 700° C. to about 990° C.; and wherein mixing is provided during crystallization.
Claim 22
Dependent Claim
62 words
The improved process of claim 19 wherein the components for forming MTiOXO 4 crystals comprise TiO 2 , K 2 HPO 4 and KHPO 4 ; and at least about 1 mole % to Ga 2 O 3 , Al 2 O 3 , SiO 2 or a mixture of Fa 2 O 3 and SiO 2 is added to the flux.
Claim 23
Dependent Claim
43 words
The improved process of claim 19 wherein the components for forming MTiOXO 4 crystals comprise KH 2 AsO 4 , KHCO 3 and TiO 2 ; and at least about l mole % of Ga 2 O 3 is added to the flux.
Claim 24
Dependent Claim
53 words
A doped single crystal of MTiOXO 4 containing at least about 100 ppm of a dopant selected from the group consisting of Ga, Al, Si or mixtures thereof, wherein M is selected from the group consisting of K, Rb and Tl and X is selected from the group consisting of P and As.
Claim 25
Dependent Claim
53 words
A doped single crystal of MTiOXO 4 containing at least about 100 ppm of a dopant selected from the group consisting of Ga, Al, Si or mixtures thereof, wherein M is selected from the group consisting of K, Rb and Tl and X is selected from the group consisting of P and As.
Claim 26
Dependent Claim
36 words
The doped single crystal of claim 22 wherein said dopant is present in an amount, at least about 200 ppm, effective to reduce the ionic conductivity of the single crystal compared to crystals without said dopant.
Claim 27
Dependent Claim
12 words
The doped single crystal of claim 23 wherein the dopant is Ga.
Claim 28
Dependent Claim
12 words
The doped single crystal of claim 23 wherein the dopant is Al.
Claim 29
Dependent Claim
12 words
The doped single crystal of claim 23 wherein the dopant is Si.
Claim 30
Dependent Claim
18 words
The doped single crystal of claim 23 in which the dopant is a mixture of Ga and Si.
Claim 31
Dependent Claim
11 words
The doped single crystal of claim 23 wherein X is P.
Claim 32
Dependent Claim
11 words
The doped single crystal of claim 23 wherein X is As.
Claim 33
Dependent Claim
11 words
The doped single crystal of claim 23 wherein M is K.
Claim 34
Dependent Claim
11 words
The doped single crystal of claim 30 wherein X is P.
Claim 35
Dependent Claim
12 words
The doped single crystal of claim 31 wherein the dopant is Ga.
Claim 36
Dependent Claim
12 words
The doped single crystal of claim 31 wherein the dopant is Al.
Claim 37
Dependent Claim
12 words
The doped single crystal of claim 31 wherein the dopant is Si.
Claim 38
Dependent Claim
17 words
The doped single crystal of claim 31 wherein the dopant is a mixture of Ga and Si.
Claim 39
Dependent Claim
11 words
The doped single crystal of claim 30 wherein X is As.
Claim 40
Dependent Claim
12 words
The doped single crystal of claim 36 wherein the dopant is Ga.
Claim 41
Dependent Claim
137 words
The doped single crystal of claim 22 wherein said single crystal is produced by preparing a substantially isothermal melt containing the components for forming MTiOXO 4 crystals and a flux comprising oxides of M and X; adding to the flux at least about 0.5 mole percent total of at least one dopant selected from the group consisting of Ga, Al and Si, calculated as the oxide and based upon the total moles of MTiOXO 4 crystals formable from the components in the melt; suspending a seed crystal of MTiOXO 4 in the melt; slowly decreasing the temperature of the melt while maintaining substantially isothermal conditions therein; and continuing decreasing the temperature until crystallization of the crystalline composition is completed while controlling the crystallizing temperature to provide a doped single crystal of MTiOXO 4 which contains said dopant.
Claim 42
Dependent Claim
137 words
The composition of claim 3 wherein the doped crystalline MTiOXO 4 is produced by preparing a substantially isothermal melt containing the components for forming MTiOXO 4 crystals and a flux comprising oxides of M and X; adding to the flux at least about 0.5 mole percent total of at least one dopant selected from the group consisting of Ga, Al and Si, calculated as the oxide and based upon the total moles of MTiOXO 4 crystals formable from the components in the melt; suspending a seed crystal of MTiOXO 4 in the melt; slowly decreasing the temperature of the melt while maintaining substantially isothermal conditions therein and continuing decreasing the temperature until crystallization of the crystalline composition is completed while controlling the crystallizing temperature to provide a doped single crystal of MTiOXO 4 which contains said dopant.
Claim 43
Dependent Claim
57 words
A composition consisting essentially of doped crystalline MTiOXO 4 wherein M is selected from the group consisting of K, Rb and Tl, and X is selected from the group consisting of P and As, said MTiOXO 4 containing at least about 100 ppm total of dopant selected from Al, Si, mixtures thereof and mixtures thereof with Ga.
Claim 44
Dependent Claim
57 words
A composition consisting essentially of doped crystalline MTiOXO 4 wherein M is selected from the group consisting of K, Rb and Tl, and X is selected from the group consisting of P and As, said MTiOXO 4 containing at least about 100 ppm total of dopant selected from Al, Si, mixtures thereof and mixtures thereof with Ga.
Claim 45
Dependent Claim
15 words
The composition of claim 40 wherein said doped crystalline MTiOXO 4 is a single crystal.
Claim 46
Dependent Claim
17 words
The composition of claim 41 containing at least about 200 ppm of said at least one dopant.
Claim 47
Dependent Claim
10 words
The composition of claim 41 wherein the dopant is Al.
Claim 48
Dependent Claim
10 words
The composition of claim 41 wherein the dopant is Si.
Claim 49
Dependent Claim
15 words
The composition of claim 41 wherein the dopant is a mixture of Ga and Si.
References Cited (Backward Citations)
US3949323A
Cited
US4231838A
Cited
US4305778A
Cited
US4746396A
Cited
US4654111A
Cited
US4761202A
Cited
JPS6340799A
Cited
US4740265A
Cited
US4766954A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1995-01-27 | 1995-07-29 | 1996-01-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1999-01-27 | 1999-07-29 | 2000-01-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2003-01-27 | 2003-07-29 | 2004-01-28 | $7700.00 | Window Closed / Lapsed |