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US4247358A
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Method of growing single crystals of alpha aluminum phosphate
Assignee: United States Department of the Army
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Filing: 1979-06-08
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Granted: 1981-01-27
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Expires: 1999-06-08
Abstract
Abstract Single crystals of alpha aluminum phosphate of high crystal perfection arerown from seeded solutions of aluminum orthophosphate and orthophosphoric acid in such a manner as to provide direct visual observation of the crystal growth process and allow precise determination of nucleation and growth kinetics. The method involves sealing the seeded solution in clear quartz ampules, inserting the ampules into a precisely temperature controlled silicone oil bath, increasing the temperature of the silicone oil bath from ambient temperature to approximately 150 degrees C. over a three hour period, programming the temperature of the bath upward at the rate of 0.1 to 2.0 degrees C. per day for periods up to sixty days, and removing the quartz ampules from the silicone oil bath and quickly cooling and removing the crystals.
Inventors
- 👤 Thomas R. AuCoin
- 👤 Abraham Schwartz
- 👤 Melvin J. Wade
- 👤 Roger J. Malik
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 09:41
CPC Classifications
C; C30; C30B; C30B7/00; C30B29/00; C30B29/10; C30B29/14
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
136 words
Method of growing single crystals of alpha aluminum phosphate of high crystal perfection from seeded solutions of aluminum orthophosphate and orthophosphoric acid in such a manner as to provide direct visual observation of the crystal growth process and allow precise determination of nucleation and growth kinetics, said method including the steps of: (A) sealing the seeded solution in clear quartz ampules, (B) inserting the ampules into a precisely temperature controlled silicone oil bath, (C) increasing the temperature of the silicone oil bath from ambient temperature to approximately 150 degrees C. over a three hour period, (D) programming the temperature of the bath upward at the rate of 0.1 to 2.0 degrees C. per day for about thirty days, and (E) removing the quartz ampules from the silicone oil bath and quickly cooling and removing the crystals.
Claim 2
Dependent Claim
136 words
Method of growing single crystals of alpha aluminum phosphate of high crystal perfection from seeded solutions of aluminum orthophosphate and orthophosphoric acid in such a manner as to provide direct visual observation of the crystal growth process and allow precise determination of nucleation and growth kinetics, said method including the steps of: (A) sealing the seeded solution in clear quartz ampules, (B) inserting the ampules into a precisely temperature controlled silicone oil bath, (C) increasing the temperature of the silicone oil bath from ambient temperature to approximately 150 degrees C. over a three hour period, (D) programming the temperature of the bath upward at the rate of 0.1 to 2.0 degrees C. per day for about thirty days, and (E) removing the quartz ampules from the silicone oil bath and quickly cooling and removing the crystals.
Claim 3
Dependent Claim
25 words
Method according to claim 1 wherein small crystals of alpha aluminum phosphate are added to the seeded solution in the quartz ampule prior to sealing.
Claim 4
Dependent Claim
40 words
Method according to claim 1 wherein the Berlinite seed crystal is cleaned by a solution of ammonium bifluoride and by exposure to a gaseous plasma prior to insertion into the ampule containing the AlPO 4 /H 3 PO 4 .
Claim 5
Dependent Claim
28 words
Method according to claim 1 wherein a teflon coated magnetic stirrer is sealed in the growth ampule for better stirring during crystal growth of the alpha aluminum phosphate.
Claim 6
Dependent Claim
19 words
Method according to claim 1 wherein the aluminum orthophosphate is replaced by aluminum hydroxide in the orthophosphoric acid solvent.
Claim 7
Dependent Claim
19 words
Method according to claim 1 wherein the aluminum orthosphosphate is replaced by sodium aluminate in the orthophosphoric acid solvent.
Claim 8
Dependent Claim
16 words
Method according to claim 1 wherein a seed of α-quartz is used instead of α-aluminum phosphate.
Claim 9
Dependent Claim
23 words
Method according to claim 1 wherein a gold wire is used to suspend the alpha aluminum phosphate seed crystal in the growth solution.
Claim 10
Dependent Claim
21 words
Method according to claim 1 wherein a platinum wire is used to suspend the Berlinite seed crystal in the growth solution.
Claim 11
Dependent Claim
12 words
Method according to claim 1 wherein the ampule is made of sapphire.
Claim 12
Dependent Claim
165 words
Method of growing single crystals of alpha aluminum phosphate of high crystal perfection in such a manner as to provide direct visual observation of the crystal growth process and allow precise determination of nucleation and growth kinetics, said method consisting of: (A) dissolving 200 grams of aluminum orthophosphate in one liter of 6 molar refluxing orthophosphoric acid at about 100 degrees C.; (B) pouring the-solution into clear quartz ampules about 8 inches tall, having a 1 inch diameter and wall thickness of 3 millimeters and containing an alpha aluminum phosphate seed crystal resting on a support plate which in turn is fused to the ampule at its center; (C) hermetically sealing the ampules; (D) immersing the ampules into a silicone oil bath contained in a pyrex jar; (E) programming the temperature of the bath upward at the rate of 0.5 degree C. per day for thirty days; and (F) removing the quartz ampule from the silicone oil bath and quickly cooling and removing the crystals.
Claim 13
Dependent Claim
165 words
Method of growing single crystals of alpha aluminum phosphate of high crystal perfection in such a manner as to provide direct visual observation of the crystal growth process and allow precise determination of nucleation and growth kinetics, said method consisting of: (A) dissolving 200 grams of aluminum orthophosphate in one liter of 6 molar refluxing orthophosphoric acid at about 100 degrees C.; (B) pouring the-solution into clear quartz ampules about 8 inches tall, having a 1 inch diameter and wall thickness of 3 millimeters and containing an alpha aluminum phosphate seed crystal resting on a support plate which in turn is fused to the ampule at its center; (C) hermetically sealing the ampules; (D) immersing the ampules into a silicone oil bath contained in a pyrex jar; (E) programming the temperature of the bath upward at the rate of 0.5 degree C. per day for thirty days; and (F) removing the quartz ampule from the silicone oil bath and quickly cooling and removing the crystals.
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) | 1984-01-27 | 1984-07-28 | 1985-01-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-01-27 | 1988-07-28 | 1989-01-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-01-27 | 1992-07-28 | 1993-01-27 | $7700.00 | Window Closed / Lapsed |