IP Library Granted Patent US 9,862,844
Granted Patent B2
US 9,862,844 · App. 15/219,450 · Granted Jan 9, 2018

Homogeneous precursor formation method and device thereof

Inventors: Rakesh Agrawal (West Lafayette, IN); Ruihong Zhang (West Lafayette, IN); Bryce Chryst Walker (Hillsboro, OR); Carol Handwerker (West Lafayette, IN)
Assignee: PURDUE RESEARCH FOUNDATION
C09D7/1233C01B19/002H01L21/0256H01L21/02557H01L21/02568H01L21/02601H01L21/02628H01L31/0326H01L31/072H01L31/1864Y02E10/50
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Quick Facts
Patent No.
US 9,862,844
App. No.
15/219,450
Granted
Jan 9, 2018
Kind
B2
Abstract

A direct solution method based on a versatile amine-thiol solvent mixture which dissolves elemental metals, metal salts, organometallic complexes, metal chalcogenides, and metal oxides is described. The metal containing and metal chalcogenide precursors can be prepared by dissolving single or multiple metal sources, chalcogens, and/or metal chalcogenide compounds separately, simultaneously, or stepwise. Multinary metal chalcogenides containing at least one of copper, zinc, tin, indium, gallium, cadmium, germanium, and lead, with at least one of sulfur, selenium, or both are obtained from the above-mentioned metal chalcogenide precursors in the form of thin films, nanoparticles, inks, etc. Furthermore, infiltration of metal containing compounds into a porous structure can be achieved using the amine-thiol based precursors. In addition, due to the appreciable solubility of metal sources, metal chalcogenides, and metal oxides in the mixture of amine(s) and thiol(s), this solvent mixture can be used to remove these materials from a system.

Claims (15)

1. A method of dissolving copper (I) sulfide (Cu 2 S), copper (II) sulfide (CuS), copper (I) selenide (Cu 2 Se), and/or copper (II) selenide (CuSe), comprising contacting Cu 2 S, CuS, Cu 2 Se and/or CuSe with a mixture of amine and dithiol to form a homogeneous solution.

2. The method of claim 1 , wherein the amine is at least one of a primary, secondary, tertiary amine, diamine, and triamine, and wherein the amine carbon chain ranges from C2 to C24.

3. The method of claim 1 , wherein the amine is a primary amine, the amine carbon chain ranges from C2 to C24.

4. The method of claim 1 , wherein the dithiol has the structure of HS-R6-SH, and wherein R6 represents at least one of an alkyl and aryl group.

5. A method of dissolving tin (II) sulfide (SnS), comprising contacting SnS with a mixture of amine and dithiol.

6. The method of claim 5 , wherein the amine is at least one of a primary, secondary, tertiary amine, diamine, and a triamine, and wherein the amine carbon chain ranges from C2 to C24.

7. The method of claim 5 , wherein the amine is a primary amine, and wherein the primary amine's carbon chain ranges from C2 to C24.

8. The method of claim 5 , wherein the dithiol has the structure of HS-R6-SH, and R6 represents at least one of any alkyl and any aryl group.

9. A method of dissolving at least one of Cu, Zn, and Sn, comprising contacting an elemental metal Cu, Zn, and/or Sn with a mixture of at least one primary amine and at least one dithiol to form a homogeneous solution.

10. The method of claim 9 , wherein the at least one primary amine is a primary amine with carbon chain ranges from C2 to C24.

11. The method of claim 9 , wherein the dithiol has the structure of HS-R6-SH, and R6 represents an alkyl and/or aryl group.

12. A method of dissolving metal oxides, comprising contacting a metal oxide with a mixture of amine and thiol to form a homogeneous solution.

13. The method of claim 12 , wherein the metal oxide comprises copper oxide, zinc oxide, tin oxide, germanium oxide, and indium oxide; in this mixture of amine and thiol.

14. The method of claim 12 , wherein the amine is a primary, secondary, tertiary amine, and/or polyamine, and the amine carbon chain ranges from C2 to C24.

15. The method of claim 12 , wherein the thiol has the structure of R5-SH and/or HS-R6-SH; R5 represents an alkane, alkene, alkyne, alcohol, or other non-carboxylic acid functional group that connects to the sulfur of the thiol group, and R6 represents an alky and/or aryl.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 14, 2017
From: AGRAWAL, RAKESH; HANDWERKER, CAROL; WALKER, BRYCE; ZHANG, RUIHONG
To: PURDUE RESEARCH FOUNDATION
Reel/Frame 044123/0001 →
CONFIRMATORY LICENSE Recorded May 31, 2017
From: PURDUE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 042642/0645 →
Continuity (3)
Continuation 14824913 · Aug 12, 2015
Provisional Application 62036233 · Aug 12, 2014
Related Publication 20160333200A1 · Nov 17, 2016