IP Library Granted Patent US 9,334,581
Granted Patent B2
US 9,334,581 · App. 13/658,591 · Granted May 10, 2016

Methods for synthesizing semiconductor quality chalcopyrite crystals for nonlinear optical and radiation detection applications and the like

Inventors: Ashley Stowe (Knoxville, TN); Arnold Burger (Nashville, TN)
Assignees: Consolidated Nuclear Security, LLC; Fisk University
C30B11/12C30B29/46
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Quick Facts
Patent No.
US 9,334,581
App. No.
13/658,591
Granted
May 10, 2016
Kind
B2
Abstract

A method for synthesizing I-III-VI 2 compounds, including: melting a Group III element; adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound; and adding a Group VI element to the single phase I-III compound under heat, with mixing, and/or via vapor transport. The Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C. Preferably, the Group I element consists of a neutron absorber and the group III element consists of In or Ga. The Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C. Preferably, the Group VI element consists of S, Se, or Te. Optionally, the method also includes doping with a Group IV element activator.

Claims (25)

1. A method for synthesizing I-III-VI 2 compounds, comprising:

melting a Group III element;

subsequently adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound;

subsequently adding a Group VI element to the single phase I-III compound and heating; and

growing a bulk crystal from the resulting I-III-VI 2 compound without using a seed crystal.

2. The method of claim 1 , wherein the Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C.

3. The method of claim 1 , wherein 1 mole of the Group I element is added to 1 mole of the Group III element.

4. The method of claim 1 , wherein the Group I element comprises a neutron absorber and the Group III element comprises one of In and Ga.

5. The method of claim 1 , wherein the Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C.

6. The method of claim 1 , wherein 2 moles of the Group VI element are added to the single phase I-III compound.

7. The method of claim 1 , wherein the Group VI element comprises one of S, Se, and Te.

8. The method of claim 1 , further comprising doping with a Group IV element activator.

9. A method for synthesizing I-III-VI Z compounds, comprising:

melting a Group III element;

subsequently adding a Group I element to the melted Group III element at a rate that allows the Group I and Group III elements to react thereby providing a single phase I-III compound;

subsequently adding a Group VI element to the single phase I-III compound under heat while mixing all constituents; and

growing a bulk crystal from the resulting I-III-VI 2 compound without using a seed crystal.

10. The method of claim 9 , wherein the Group III element is melted at a temperature of between about 200 degrees C. and about 700 degrees C.

11. The method of claim 9 , wherein 1 mole of the Group I element is added to 1 mole of the Group III element.

12. The method of claim 9 , wherein the Group I element comprises a neutron absorber and the Group III element comprises one of In and Ga.

13. The method of claim 9 , wherein the Group VI element and the single phase I-III compound are heated to a temperature of between about 700 degrees C. and about 1000 degrees C.

14. The method of claim 9 , wherein 2 moles of the Group VI element are added to the single phase I-III compound.

15. The method of claim 9 , wherein the Group VI element comprises one of S, Se, and Te.

16. The method of claim 9 , further comprising doping with a Group IV element activator.

17. The method of claim 9 , wherein mixing all constituents comprises rotating all constituents at an angle.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 25, 2015
From: BABCOCK & WILCOX TECHNICAL SERVICES Y-12, LLC
To: CONSOLIDATED NUCLEAR SECURITY, LLC
Reel/Frame 035252/0604 →
CONFIRMATORY LICENSE Recorded Oct 28, 2013
From: B&W Y-12, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 031505/0395 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2012
From: BURGER, ARNOLD
To: FISK UNIVERSITY
Reel/Frame 029177/0028 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 23, 2012
From: STOWE, ASHLEY
To: BABCOCK & WILCOX TECHNICAL SERVICES Y-12, L.L.C.
Reel/Frame 029177/0123 →
Continuity (1)
Related Publication 20140144373A1 · May 29, 2014