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US 11,453,585 B2Granted
Formation of high quality alane
AssigneeSavannah River Nuclear Solutions, LLC
InventorsRagaiy Zidan, Christopher S. McWhorter, Patrick A. Ward
Life of this patent
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Abstract
Methods for forming alane are described. The method includes addition of toluene at a temperature above the crystallization temperature of alane to a lower temperature solution that includes alane adduct, ether, and toluene. Upon the addition, a crystallization mixture is formed that is at or near the crystallization temperature of alane. The alane of the mixture crystallizes over a period of time to form a high purity alane polymorph.
Claims19
A method for forming alane comprising:
- combining an alane adduct, an ether, and a first amount of toluene to form a liquid mixture, the liquid mixture including the ether in an amount of from about 1 vol. % to about 50 vol. %;
- adding a second amount of toluene to the liquid mixture to form a crystallization mixture, wherein at the addition, the liquid mixture is at a temperature of from about 15° C. to about 45° C. and the second amount of toluene is at a temperature that is greater than the crystallization temperature of the alane, wherein upon the addition, the crystallization mixture thus formed is at a temperature of from about 70° C. to about 80° C.;
- and
- maintaining the crystallization mixture at a temperature of from about 70° C. to about 80° C. for a period of from about 2 hours to about 5 hours, the alane of the alane adduct polymerizing during the period.
1 more element
A method for forming α-alane comprising:
- combining an alane adduct, an ether, and a first amount of toluene to form a liquid mixture, the liquid mixture including the ether in an amount of from about 1 vol. % to about 15 vol. %;
- adding a second amount of toluene to the liquid mixture to form a crystallization mixture, wherein at the addition, the liquid mixture is at a temperature of from about 15° C. to about 45° C. and the second amount of toluene is at a temperature of from about 85° C. to about 110°, wherein upon the addition, the crystallization mixture thus formed is at a temperature of from about 70° C. to about 80° C.;
- maintaining the crystallization mixture at a temperature of from about 70° C. to about 80° C. for a period of from about 3 hours to about 5 hours;
- and
- distilling the ether from the crystallization mixture during the period, the alane of the alane adduct polymerizing during the period, the polymerized alane comprising α-alane in an amount of about 99% or greater.
2 more elements
Dependencies are inferred from the claim text.