US4043860A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Method of growing single crystals of neodymium pentaphosphate
Assignee: United States Department of the Army
•
Filing: 1977-01-24
•
Granted: 1977-08-23
•
Expires: 1997-01-24
Abstract
Abstract Single crystals of neodymium pentaphosphate greater than one centimeter in size and of high purity and quality are grown from polyphosphoric acid solutions using the combination of a dilute solution, seeding, growth temperatures of 500° to 650° C, and a double crucible configuration.
Inventors
- 👤 Thomas R. Au Coin
- 👤 Abraham Schwartz
- 👤 John G. Gualtieri
- 👤 Melvin J. Wade
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 17:32
CPC Classifications
C; C30; C30B; C30B7/00; C30B29/00; C30B29/10; C30B29/14; Y; Y10; Y10S; Y10S117/00; Y10S117/90
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
203 words
Method of growing single crystals of neodymium pentaphosphate greater than 1 centimeter in size and of high purity and quality from polyphosphoric acid solutions, said method including the steps of A. heating orthophosphoric acid contained in a first crucible made of a material that is leakproof and highly resistant to acid attack to about 200° C, B. adding neodymium oxide to the acid in the ratio of 0.5 to 3.0 grams of oxide per 50 milliliters of orthophosphoric acid, C. increasing the temperature to a temperature of about 350° C, D. placing the first crucible in a second crucible, larger than the first crucible, said second crucible containing phosphoric acid and being made of a material that is leakproof and highly resistant to acid attack, E. placing lids over said first and second crucibles, and heating the double crucible configuration in a furnace at a temperature of about 500° C to 650° C for about 24 to 48 hours, F. removing the lids from said crucibles and adding several seed crystals to said first crucible, and G. replacing the lids on the crucibles and maintaining the furnace at about 500° C to 650° C until maximum growth of the single crystals are obtained.
Claim 2
Dependent Claim
203 words
Method of growing single crystals of neodymium pentaphosphate greater than 1 centimeter in size and of high purity and quality from polyphosphoric acid solutions, said method including the steps of A. heating orthophosphoric acid contained in a first crucible made of a material that is leakproof and highly resistant to acid attack to about 200° C, B. adding neodymium oxide to the acid in the ratio of 0.5 to 3.0 grams of oxide per 50 milliliters of orthophosphoric acid, C. increasing the temperature to a temperature of about 350° C, D. placing the first crucible in a second crucible, larger than the first crucible, said second crucible containing phosphoric acid and being made of a material that is leakproof and highly resistant to acid attack, E. placing lids over said first and second crucibles, and heating the double crucible configuration in a furnace at a temperature of about 500° C to 650° C for about 24 to 48 hours, F. removing the lids from said crucibles and adding several seed crystals to said first crucible, and G. replacing the lids on the crucibles and maintaining the furnace at about 500° C to 650° C until maximum growth of the single crystals are obtained.
Claim 3
Dependent Claim
27 words
Method according to claim 1 wherein the neodymium pentaphosphate is diluted with a cation selected from the group consisting of yttrium, indium, bismuth, gadolinium, cerium, and lanthanum.
Claim 4
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with yttrium.
Claim 5
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with indium.
Claim 6
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with bismuth.
Claim 7
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with gadolinium.
Claim 8
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with cerium.
Claim 9
Dependent Claim
13 words
Method according to claim 2 wherein the neodymium pentaphosphate is diluted with lanthanum.
Claim 10
Dependent Claim
39 words
Method according to claim 1 wherein the crucible that is leakproof and highly resistant to acid attack is of a material selected from the group consisting of vitreous carbon, pyrolytic carbon coated carbon and pyrolytic silicon carbide coated carbon.
Claim 11
Dependent Claim
11 words
Method according to claim 9 wherein the material is vitreous carbon.
Claim 12
Dependent Claim
13 words
Method according to claim 9 wherein the material is pyrolytic carbon coated carbon.
Claim 13
Dependent Claim
14 words
Method according to claim 9 wherein the material is pyrolytic silicon carbide coated carbon.
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) | 1980-08-22 | 1981-02-21 | 1981-08-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-08-22 | 1985-02-21 | 1985-08-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-08-22 | 1989-02-21 | 1989-08-23 | $7700.00 | Window Closed / Lapsed |