US3904736A
Expired / Lapsed
US
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Preparing microspheres of actinide nitrides from carbon containing oxide sols
Assignee: WR Grace and Co
•
Filing: 1966-06-01
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Granted: 1975-09-09
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Expires: 1986-06-01
Abstract
Abstract A process for preparing uranium nitride, uranium oxynitride and uranium carboxynitride microspheres and the microspheres as compositions of matter. The microspheres are prepared from carbide sols by reduction and nitriding steps.
Inventors
- 👤 Leonard V Triggiani
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 11:37
CPC Classifications
G; G21; G21C; G21C3/00; G21C3/42; G21C3/58; G21C3/62; C; C01; C01B; C01B21/00; C01B21/06; C01B21/0615; C01B21/063; C01B21/082; C01B21/0821; C01B21/0828; G21C3/626; C01P; C01P2002/00; C01P2002/70; C01P2002/77; C01P2004/00; C01P2004/30; C01P2004/32; C01P2004/60; C01P2004/61; C01P2006/00; C01P2006/80; Y; Y02; Y02E; Y02E30/00; Y02E30/30
Claims Analysis
Total Claims: 27
Claim 1
Independent Claim
136 words
A PROCESS FOR PREPARING NITRIDES, OXYNITRIDES, AND CALBOXYNITRIDES OF ACTINIDE METALS AND MIXTUES OF ACTINIDE METALS WITH OTHER IONS IN MICROSPHEROIDAL FORM, WHICH COMPRISES: A. PEPARING CARBON CONTAINING SPHERES OF SAID ACTINIDE METAL FROM THE CORRESPONDING ACTINIDE METAL OXIDE SOL WHEREIN THE CARBON TO ACTINIDE METAL RATIO IS IN THE RANGE OF 2.2 TO 2.4, LESS THAN 2.1, GREATER THAN 2.4 TO ABOUT 4.4 RESPECTIVELY, B. HEATING SAID SPHERES TO A TEMPERATURE OF ABOUT 400*-600*C. IN A REDUCING GAS ATMOSPHERE TO REMOVE EXCESS OXYGEN, C. SINTERING HE SPHERES AT A TEMPERATURE OF ABOU 1400* TO 1500*C. IN A INERT ATMOSPHERE TO COMPLETE CARBIDE FORMATION, D. CONVERTING THE CARBIDE SPHERES TO THE NITRIDE BY HEATING IN A NITROGEN ATMOSPHERE, E. DENSIFYING THE NITRIDE SPHERES BY HEATING IN AN INERT ATMOSPHERE, AND F. RECOVERING THE NITRIDE MICROSPHERE PRODUCT.
Claim 2
Dependent Claim
136 words
A PROCESS FOR PREPARING NITRIDES, OXYNITRIDES, AND CALBOXYNITRIDES OF ACTINIDE METALS AND MIXTUES OF ACTINIDE METALS WITH OTHER IONS IN MICROSPHEROIDAL FORM, WHICH COMPRISES: A. PEPARING CARBON CONTAINING SPHERES OF SAID ACTINIDE METAL FROM THE CORRESPONDING ACTINIDE METAL OXIDE SOL WHEREIN THE CARBON TO ACTINIDE METAL RATIO IS IN THE RANGE OF 2.2 TO 2.4, LESS THAN 2.1, GREATER THAN 2.4 TO ABOUT 4.4 RESPECTIVELY, B. HEATING SAID SPHERES TO A TEMPERATURE OF ABOUT 400*-600*C. IN A REDUCING GAS ATMOSPHERE TO REMOVE EXCESS OXYGEN, C. SINTERING HE SPHERES AT A TEMPERATURE OF ABOU 1400* TO 1500*C. IN A INERT ATMOSPHERE TO COMPLETE CARBIDE FORMATION, D. CONVERTING THE CARBIDE SPHERES TO THE NITRIDE BY HEATING IN A NITROGEN ATMOSPHERE, E. DENSIFYING THE NITRIDE SPHERES BY HEATING IN AN INERT ATMOSPHERE, AND F. RECOVERING THE NITRIDE MICROSPHERE PRODUCT.
Claim 3
Dependent Claim
43 words
The process according to claim 1 wherein the product is the nitride, the actinide metal selected from the group consisting of thorium, uranium, and plutonium, and the carbon to actinide metal ratio used in preparing the carbon containing spheres is 2.2 to 2.4.
Claim 4
Dependent Claim
16 words
HEating the spheres in an argon atmosphere at an elevated temperature to form the actinide carbide;
Claim 5
Dependent Claim
16 words
HEating the spheres in an argon atmosphere at an elevated temperature to form the actinide carbide;
Claim 6
Dependent Claim
22 words
And thereafter heating the resulting carbide in a nitrogen atmosphere at a temperature of about 1500*C to form said actinide mononitride microspheres.
Claim 7
Dependent Claim
22 words
And thereafter heating the resulting carbide in a nitrogen atmosphere at a temperature of about 1500*C to form said actinide mononitride microspheres.
Claim 8
Dependent Claim
28 words
The process according to claim 1 wherein the oxygen removal is effected by heating the spheres in a hydrogen atmosphere at a temperature of about 400*C. to 600*C.
Claim 9
Dependent Claim
25 words
The process according to claim 1 wherein the spheres are heated to about 1100*C. to 1800*C. for 10 to 30 hours to complete carbide formation.
Claim 10
Dependent Claim
54 words
The process according to claim 1 wherein the nitride is formed from the caRbide microspheres in a nitrogen atmosphere wherein the nitrogen is swept through the reactor at rate in excess of 1 liter per minute per 10 grams of carbide spheres, and the reactor is maintained at a temperature of 1450* to 1850*C.
Claim 11
Dependent Claim
32 words
The process according to claim 1 wherein the nitride is densified by heating in an atmosphere of an inert gas at a temperature of 1800* to 2000*C. for 0.1 to 1 hour.
Claim 12
Dependent Claim
12 words
The process according to claim 1 wherein the actinide metal is thorium.
Claim 13
Dependent Claim
12 words
The process according to claim 1 wherein the actinide metal is uranium.
Claim 14
Dependent Claim
12 words
The process according to claim 1 wherein the actinide metal is plutonium.
Claim 15
Dependent Claim
49 words
The process according to claim 1 wherein the product has the empirical formula XNOC wherein X is an actinide metal selected from the group consisting of thoria, urania and plutonia, and the carbon to actinide metal ratio used in preparing the spheres is above about 2.4 to about 4.4.
Claim 16
Dependent Claim
47 words
The process according to claim 1 wherein the product has the empirical formula XNO wherein X is an actinide metal selected from the group consisting of thoria, urania, and plutonia, and the actinide metal to carbon ratio used in preparing the spheres is less than about 2.1.
Claim 17
Dependent Claim
84 words
A process for converting actinide prepared from colloidal materials to nitrides which comprises: a. Preparing carbon containing actinide oxide microspheres by mixing carbon and actinide metal sols and drying to form microspheres; b. Heating said microspheres in a reducing atmosphere to remove excess oxygen; c. Sintering the spheres to complete carbide formation; d. Converting the carbide spheres to the nitride by heating in a nitrogen atmosphere; e. Densifying the nitride spheres by heating in an inert atmosphere and; f. Recovering the nitride microspheres product.
Claim 18
Dependent Claim
84 words
A process for converting actinide prepared from colloidal materials to nitrides which comprises: a. Preparing carbon containing actinide oxide microspheres by mixing carbon and actinide metal sols and drying to form microspheres; b. Heating said microspheres in a reducing atmosphere to remove excess oxygen; c. Sintering the spheres to complete carbide formation; d. Converting the carbide spheres to the nitride by heating in a nitrogen atmosphere; e. Densifying the nitride spheres by heating in an inert atmosphere and; f. Recovering the nitride microspheres product.
Claim 19
Dependent Claim
39 words
The process according to claim 12 wherein the actinide metal is selected from the group consisting of thoria, urania and plutonia and the carbon to actinide metal ratio used to prepare the carbon containing spheres is 2.2 to 2.4.
Claim 20
Dependent Claim
114 words
A process for preparing nitrides, oxynitrides, and carboxynitrides of actinide metals and actinide metals with other ions which comprises: a. Preparing carbon containing colloidal residues of said actinide metal oxide from the corresponding actinide oxide sol, wherein the carbon to actinide metal ratio is 2.2 to 2.4, less than 2.1 and 2.4 to about 4.4 respectively, b. Preparing spheres of said residues, c. Heating said residue in a reducing gas atmosphere to remove excess oxygen, d. Sintering the residues to complete carbide formation, e. Converting the carbide residues to the nitrides by heating in a nitrogen atmosphere, f. Densifying the nitride residues by heating in an inert atmosphere, and g. Recovering the nitride product.
Claim 21
Dependent Claim
114 words
A process for preparing nitrides, oxynitrides, and carboxynitrides of actinide metals and actinide metals with other ions which comprises: a. Preparing carbon containing colloidal residues of said actinide metal oxide from the corresponding actinide oxide sol, wherein the carbon to actinide metal ratio is 2.2 to 2.4, less than 2.1 and 2.4 to about 4.4 respectively, b. Preparing spheres of said residues, c. Heating said residue in a reducing gas atmosphere to remove excess oxygen, d. Sintering the residues to complete carbide formation, e. Converting the carbide residues to the nitrides by heating in a nitrogen atmosphere, f. Densifying the nitride residues by heating in an inert atmosphere, and g. Recovering the nitride product.
Claim 22
Dependent Claim
40 words
The process according to claim 14 wherein the product is the nitride, the actinide metal oxide is selected from the group consisting of oxides of thorium, uranium, and plutonium and the carbon to actinide metal ratio is 2.2 to 2.4.
Claim 23
Dependent Claim
62 words
The process according to claim 14 wherein the oxygen removal is effected by heating the residues in a hydrogen atmosphere of a temperature of about 400* to 600*C, carbide formation is completed by heating the residues to 1100* to 1300*C for about 10 to 30 hours and the nitride is formed in a nitrogen atmosphere at a temperature of 1450* to 1850*C.
Claim 24
Dependent Claim
12 words
A process for preparing crystalline microspheres consisting essentially of actinide mononitride comprising:
Claim 25
Dependent Claim
12 words
A process for preparing crystalline microspheres consisting essentially of actinide mononitride comprising:
Claim 26
Dependent Claim
88 words
A process for preparing crystalline microspheres consisting essentially of actinide mononitride comprising: a. preparing carbon containing actinide oxide microspheres having a carbon to actinide metal ratio of about 2.3 to 1 by mixing carbon and actinide metal oxide sols and drying to form microspheres; b. heating the spheres in an argon atmosphere at an elevated temperature to form the actinide carbide; c. and thereafter heating the resulting carbide in a nitrogen atmosphere at an elevated temperature at which said carbide is readily converted to said actinide mononitride microspheres.
Claim 27
Dependent Claim
88 words
A process for preparing crystalline microspheres consisting essentially of actinide mononitride comprising: a. preparing carbon containing actinide oxide microspheres having a carbon to actinide metal ratio of about 2.3 to 1 by mixing carbon and actinide metal oxide sols and drying to form microspheres; b. heating the spheres in an argon atmosphere at an elevated temperature to form the actinide carbide; c. and thereafter heating the resulting carbide in a nitrogen atmosphere at an elevated temperature at which said carbide is readily converted to said actinide mononitride microspheres.
References Cited (Backward Citations)
US3228748A
Cited
US3213032A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-09-08 | 1979-03-10 | 1979-09-09 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-09-08 | 1983-03-10 | 1983-09-09 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-09-08 | 1987-03-10 | 1987-09-09 | $7700.00 | Window Closed / Lapsed |