Hydrothermal method for growth of alkaline earth metal stannate bulk single crystals and crystals formed thereby

Patent metadata

Field	Value
Publication number	US-11840772-B2
Application number	US-202217584807-A
Country	US
Kind code	B2
Filing date	Jan 26, 2022
Priority date	Jan 26, 2021
Publication date	Dec 12, 2023
Grant date	Dec 12, 2023

Abstract

Hydrothermal methods for the synthesis of bulk crystals of alkaline earth metal stannates are described. Methods can be utilized for growth of large, single crystals of alkaline earth metal stannates including fully cubic BaSnO3 and SrSnO3.

First claim

What is claimed is:

1. A method for forming a crystal comprising an alkaline earth metal stannate comprising:
heating and pressurizing an aqueous solution held within a reactor to develop a temperature differential between a first zone of the reactor and a second zone of the reactor, the aqueous solution containing a mineralizer, the first zone of the reactor containing an alkaline earth metal source and a tetravalent tin source, wherein upon the heating and pressurizing, growth of a crystal comprising cubic alkaline earth metal stannate is initiated in the second zone of the reactor; and
maintaining the heating and pressurizing within the reactor for a growth period to form a single crystal comprising the alkaline earth metal stannate, the single crystal defining a width that is about 1 mm or greater and a thickness that is about 1 mm or greater.

2. The method of claim 1 , wherein the reactor comprises a liner comprising a noble metal.

3. The method of claim 2 , wherein the noble metal is platinum.

4. The method of claim 1 , wherein the alkaline earth metal source is a hydroxide of the alkaline earth metal.

5. The method of claim 1 , wherein the alkaline earth metal comprises barium or strontium.

6. The method of claim 1 , wherein the tetravalent tin source comprises stannic oxide.

7. The method of claim 1 , further comprising locating a seed crystal comprising the alkaline earth metal stannate in the reactor prior to the heating and pressurizing.

8. The method of claim 1 , wherein the mineralizer comprises cesium hydroxide at a concentration of from about 0.5 M to about 25 M.

9. The method of claim 1 , the first zone of the reactor further comprising a dopant source.

10. The method of claim 9 , wherein the dopant of the dopant source is a trivalent ion (n-doping).

11. The method of claim 10 , wherein the dopant comprises lanthanum.

12. The method of claim 9 where the dopant of the dopant source is a monovalent ion (p-doping).

13. The method of claim 12 , wherein the dopant comprises silver.

14. The method of claim 1 , wherein the aqueous solution is pressurized to a pressure between about 50 MPa and about 200 MPa.

15. The method of claim 1 , wherein the aqueous solution is heated to a temperature of about 750° C. or less.

16. The method of claim 1 , wherein the temperature differential is from about 20° C. to about 40° C.

17. A single crystal comprising fully cubic strontium stannate, wherein the single crystal defines a width that is about 1 mm or greater and a thickness that is about 1 mm or greater.

18. The single crystal of claim 17 , wherein the single crystal consists of the fully cubic strontium stannate.

19. The single crystal of claim 17 , further comprising a dopant.

20. The single crystal of claim 19 , the dopant comprising a trivalent ion.

21. The single crystal of claim 20 , the dopant comprising lanthanum.

22. The single crystal of claim 19 , the dopant comprising a monovalent ion.

23. The single crystal of claim 22 , the dopant comprising silver.

Assignees

• Univ Clemson
• Univ Clemson Res Foundation

Inventors

• Kolis Joseph W
• Terry Rylan J
• Mcmillen Colin D

Classifications

• C30B29/22 Primary

  Complex oxides · CPC title

• C30B7/005

  Epitaxial layer growth · CPC title

• C30B7/04

  using aqueous solvents · CPC title

• C30B7/10

  by application of pressure, e.g. hydrothermal processes · CPC title