Method of synthesising nitride nanocrystals

Patent metadata

Field	Value
Publication number	US-9938148-B2
Application number	US-201314440048-A
Country	US
Kind code	B2
Filing date	Nov 12, 2013
Priority date	Nov 13, 2012
Publication date	Apr 10, 2018
Grant date	Apr 10, 2018

Abstract

A method of producing nitride nanoparticles comprises reacting at least one organometallic compound, for example an alkyl metal, with at least one source of nitrogen. The reaction may involve one or more liquid phase organometallic compounds, or may involve one or more liquid phase organometallic compounds dissolved in a solvent or solvent mixture. The reaction constituents may be heated to a desired reaction temperature (for example in the range 40° C. to 300° C.).

First claim

The invention claimed is:

1. A method of producing nitride nanoparticles, the method comprising: reacting at least one source of nitrogen with at least one organometallic compound at a reaction temperature less than 300° C., the reaction producing the nitride nanoparticles, the at least one source of nitrogen comprising ammonia or a metal amide, and the organometallic compound(s) being either in a liquid phase or in liquid solution.

2. A method as claimed in claim 1 and comprising reacting the at least one organometallic compound and the at least one source of nitrogen in at least one solvent.

3. A method as claimed in claim 2 and comprising reacting the at least one organometallic compound and the at least one source of nitrogen in a solvent mixture comprising at least two solvents.

4. A method as claimed in claim 3 wherein at least one of the solvents in the solvent mixture provides a ligand for the nitride nanoparticles.

5. A method as claimed in claim 2 , wherein the at least one solvent comprises an aprotic solvent.

6. A method as claimed in claim 2 and comprising disposing the at least organometallic compound and the at least one source of nitrogen in the at least one solvent to form a reaction mixture.

7. A method as claimed in claim 6 , and comprising, at a first time, disposing a first quantity of the or each organometallic compound in the at least one solvent and, at a second time later than the first time, disposing a second quantity of the or each organometallic compound in the at least one solvent.

8. A method as claimed in claim 6 , wherein the reaction temperature is greater than 200° C., and wherein the at least one source of nitrogen comprises the ammonia.

9. A method as claimed in claim 6 , wherein the reaction temperature is less than 200° C., and wherein the at least one source of nitrogen comprises the metal amide.

10. A method as claimed in claim 2 and comprising disposing the at least one organometallic compound in the at least one solvent to form a reaction mixture, and passing the at least one source of nitrogen through the reaction mixture.

11. A method as claimed in claim 10 , and comprising, at a first time, disposing a first quantity of the or each organometallic compound in the at least one solvent and, at a second time later than the first time, disposing a second quantity of the or each organometallic compound in the at least one solvent.

12. A method as claimed in claim 11 , wherein the at least one source of nitrogen consists solely of ammonia gas, and wherein the molar quantity of the first and any subsequent addition of the or each organometallic compound is at least 2% of the molar quantity of ammonia passing through the reaction mixture per minute.

13. A method as claimed in claim 11 , wherein the at least one source of nitrogen consists solely of ammonia gas, and wherein the molar quantity of the first and any subsequent addition of the or each organometallic compound is no more than twice of the molar quantity of ammonia passing through the reaction mixture per minute.

14. A method as claimed in claim 10 , wherein the reaction temperature is less than 200° C., and wherein the at least one source of nitrogen comprises the metal amide.

15. A method as claimed in claim 10 , wherein the reaction temperature is greater than 200° C., and wherein the at least one source of nitrogen comprises the ammonia.

16. A method as claimed in claim 2 , wherein the at least one source of nitrogen consists solely of ammonia gas, and wherein the volume of ammonia per minute passed through the reaction mixture is greater than 1% of the volume of the reaction mixture.

17. A method as claimed in claim 2 , wherein the at least one source of nitrogen consists solely of ammonia gas, and wherein the volume of ammonia per minute passed through the reaction mixture is less than the volume of the reaction mixture.

18. A method as claimed in claim 1 , wherein the reaction directly produces the nitride nanoparticles without an intermediate calcination step.

19. A method of producing nitride nanoparticles, the method comprising: reacting at least one source of nitrogen with at least one organometallic compound at a reaction temperature less than 300° C., the reaction producing the nitride nanoparticles, the organometallic compound(s) being either in a liquid phase or in liquid solution, wherein the at least one organometallic compound comprises at least one alkyl metal compound, and wherein the at least one alkyl metal compound comprises one or more of: diethylzinc, triethylaluminium and trimethylindium.

20. A method as claimed in claim 19 , wherein the at least one source of nitrogen comprising ammonia or a metal amide.

Assignees

• Sharp Kk

Inventors

• Grundy Alastair James Daniel
• Taylor Peter Neil
• Schreuder Michael Alan
• Hooper Stewart Edward
• Heffernan Jonathan

Classifications

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C30B29/60

  characterised by shape · CPC title

• C09K11/62

  containing gallium, indium or thallium · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01B21/0637

  with metals not specified in groups C01B21/0607 - C01B21/0635, other than aluminium, titanium, zirconium or hafnium · CPC title