IP Library Granted Patent US 8,425,865
Granted Patent B2
US 8,425,865 · App. 13/140,810 · Granted Apr 23, 2013

Method of synthesizing pyrite nanocrystals

Inventors: Cyrus Wadia (Alexandria, VA); Yue Wu (West Lafayette, IN)
Assignee: The Regents of the University of California
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Quick Facts
Patent No.
US 8,425,865
App. No.
13/140,810
Granted
Apr 23, 2013
Kind
B2
Abstract

A method of synthesizing pyrite nanocrystals is disclosed which in one embodiment includes forming a solution of iron (III) diethyl dithiophosphate and tetra-alkyl-ammonium halide in water. The solution is heated under pressure. Pyrite nanocrystal particles are then recovered from the solution.

Claims (41)

1. A method of synthesizing pyrite nanocrystals comprising:

forming a solution of a molecular precursor and tetra-alkyl-ammonium halide in water;

heating the solution under pressure; and

recovering pyrite nanocrystal particles from the solution.

2. The method of claim 1 wherein the tetra-alkyl-ammonium halide is alkyl-trimethyl-ammonium.

3. The method of claim 2 wherein an alkyl group of the alkyl-trimethyl-ammonium halide is ethyl.

4. The method of claim 2 wherein an alkyl group of the alkyl-trimethyl-ammonium halide is hexadecyl-trimethyl-ammonium halide.

5. The method of claim 4 wherein a halide group of the hexadecyl-trimethyl-ammonium halide is selected from the group consisting of fluoride, chloride, bromide, and iodide.

6. The method of claim 1 wherein the molecular precursor is selected from a group consisting of iron (III) diethyl dithiophosphate, a radical thereof, and a combination of both the iron (III) diethyl dithiophosphate and the radical thereof.

7. The method of claim 6 further comprising forming the molecular precursor in a reaction between iron (III) chloride and diethyl dithiophosphate ammonium salt.

8. The method of claim 7 wherein forming the molecular precursor comprises:

forming a precursor solution of the iron (III) chloride and the diethyl dithiophosphate ammonium salt; and

drying the solution.

9. The method of claim 8 wherein forming the solution comprises adding the molecular precursor and the tetra-alkyl-ammonium halide to the water.

10. The method of claim 7 wherein forming the solution comprises:

forming an aqueous precursor solution of the iron (III) chloride and the diethyl dithiophosphate which react to produce the iron (III) diethyl dithiophosphate; and

adding the tetra-alkyl-ammonium halide to the aqueous precursor solution.

11. The method of claim 6 wherein forming the solution comprises:

forming a precursor solution of the molecular precursor in the water;

forming a tetra-alkyl-ammonium halide solution of the tetra-alkyl-ammonium halide and the water; and

mixing the precursor and tetra-alkyl-ammonium halide solutions.

12. The method of claim 11 further comprising agitating the tetra-alkyl-ammonium halide solution prior to mixing the precursor and tetra-alkyl-ammonium halide solutions.

13. The method of claim 12 further comprising agitating the solution while mixing the precursor and tetra-alkyl-ammonium halide solutions.

14. The method of claim 11 further comprising sonicating the tetra-alkyl-ammonium halide solution prior to mixing the precursor and tetra-alkyl-ammonium halide solutions.

15. The method of claim 14 further comprising sonicating the solution while mixing the precursor and tetra-alkyl-ammonium halide solutions.

16. The method of claim 1 wherein heating the solution comprises heating the solution to a temperature above 150° C.

17. The method of claim 1 wherein heating the solution comprises heating the solution to a temperature of at least about 180° C.

18. The method of claim 1 wherein heating the solution comprises heating the solution to a temperature of at least about 200° C.

19. The method of claim 1 wherein the pressure during heating the solution reaches at least about 150 psi.

20. The method of claim 1 wherein the pressure during heating the solution reaches at least about 165 psi.

21. The method of claim 1 wherein the pressure during heating the solution reaches at least about 180 psi.

22. The method of claim 1 wherein a ph of the solution is within the range of 3 and above.

23. The method of claim 1 wherein forming the solution further comprises adding an amine to the solution.

24. The method of claim 23 wherein the amine is olyelamine.

25. The method of claim 2 wherein an alkyl group of the alkyl-trimethyl-ammonium halide is a carbon chain alkyl that is longer than ethyl.

26. The method of claim 2 wherein an alkyl group of the alkyl-trimethyl-ammonium halide is a carbon chain alkyl that is longer than hexadecyl-trimethyl-ammonium.

27. The method of claim 7 wherein forming the solution comprises:

forming an aqueous precursor solution of the iron (III) chloride and the diethyl dithiophosphate which react to produce the radical thereof; and

adding the tetra-alkyl-ammonium halide to the aqueous precursor solution.

28. The method of claim 12 further comprising agitating the solution after mixing the precursor and tetra-alkyl-ammonium halide solutions.

29. The method of claim 14 further comprising sonicating the solution after mixing the precursor and tetra-alkyl-ammonium halide solutions.

Assignments (2)
CONFIRMATORY LICENSE Recorded Sep 14, 2011
From: REGENTS OF THE UNIVERSITY OF CALIFORNIA, THE
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 026916/0020 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 31, 2011
From: WADIA, CYRUS; WU, YUE
To: THE REGENTS OF THE UNIVERSITY OF CALIFORNIA
Reel/Frame 026840/0783 →
Continuity (2)
Provisional Application 61139485 · Dec 19, 2008
Related Publication 20110305626A1 · Dec 15, 2011