IP Library Granted Patent US 9,163,324
Granted Patent B2
US 9,163,324 · App. 13/427,058 · Granted Oct 20, 2015

Method for producing nitride crystal

Inventors: Hideo Fujisawa (Ibaraki, JP); Yutaka Mikawa (Ibaraki, JP); Kazunori Kamada (Ibaraki, JP)
Assignee: MITSUBISHI CHEMICAL CORPORATION
C30B7/10C30B7/105C30B29/403C30B29/406
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Quick Facts
Patent No.
US 9,163,324
App. No.
13/427,058
Granted
Oct 20, 2015
Kind
B2
Abstract

A method for producing a nitride crystal, comprising growing a nitride crystal on the surface of a seed crystal put in a reactor while the temperature and the pressure inside the reactor that contains, as put thereinto, a seed crystal having a hexagonal-system crystal structure, a nitrogen-containing solvent, a starting material, and a mineralizing agent containing fluorine and at least one halogen element selected from chlorine, bromine and iodine are so controlled that the solvent therein could be in a supercritical state and/or a subcritical state to thereby grow a nitride crystal on the surface of the seed crystal in the reactor.

Claims (22)

1. A method for producing a gallium nitride crystal, comprising:

placing in a reactor a starting material which comprises at least one of metal gallium and a nitride including gallium;

placing a seed crystal in the reactor; and

growing a gallium nitride crystal on a surface of the seed crystal in a presence of a nitrogen-containing solvent and a mineralizing agent,

wherein the growing of the gallium nitride crystal comprises controlling a temperature and a pressure inside the reactor such that the nitrogen-containing solvent is in a supercritical state and/or a subcritical state, the mineralizing agent includes fluorine and at least one halogen element selected from the group consisting of chlorine, bromine and iodine, when the mineralizing agent includes chlorine and fluorine, a molar concentration of chlorine is at least 5 times a molar concentration of fluorine in the mineralizing agent, when the mineralizing agent includes bromine and fluorine, a molar concentration of bromine is at least 0.5 times a molar concentration of fluorine in the mineralizing agent, and when the mineralizing agent includes iodine and fluorine, a molar concentration of iodine is at least 0.5 times a molar concentration of fluorine in the mineralizing agent.

2. The method for producing a gallium nitride crystal of claim 1 , wherein the mineralizing agent contains chlorine and fluorine.

3. The method for producing a gallium nitride crystal of claim 2 , wherein the molar concentration of chlorine in the mineralizing agent is from 10 to 200 times the molar concentration of fluorine in the mineralizing agent.

4. The method for producing a gallium nitride crystal of claim 3 , wherein a total molar amount of the at least one halogen element contained in the mineralizing agent is from 0.1 to 30 mol % of a molar amount of the nitrogen-containing solvent.

5. The method for producing a gallium nitride crystal of claim 1 , wherein the mineralizing agent contains bromine and fluorine.

6. The method for producing a gallium nitride crystal of claim 5 , wherein the molar concentration of bromine in the mineralizing agent is from 1 to 100 times the molar concentration of fluorine in the mineralizing agent.

7. The method for producing a gallium nitride crystal of claim 6 , wherein a total molar amount of the at least one halogen element contained in the mineralizing agent is from 0.1 to 30 mol % of a molar amount of the nitrogen-containing solvent.

8. The method for producing a gallium nitride crystal of claim 1 , wherein the mineralizing agent contains iodine and fluorine.

9. The method for producing a gallium nitride crystal of claim 8 , wherein the molar concentration of iodine in the mineralizing agent is from 1 to 100 times the molar concentration of fluorine in the mineralizing agent.

10. The method for producing a gallium nitride crystal of claim 9 , wherein a total molar amount of the at least one halogen element contained in the mineralizing agent is from 0.1 to 30 mol % of a molar amount of the nitrogen-containing solvent.

11. The method for producing a gallium nitride crystal of claim 1 , wherein a total molar amount of the at least one halogen element contained in the mineralizing agent is from 0.1 to 30 mol % of a molar amount of the nitrogen-containing solvent.

12. The method for producing a gallium nitride crystal of claim 1 , wherein the starting material is melted inside the reactor in a region having a temperature which is higher than a temperature of a region in which the gallium nitride crystal is grown on the surface of the seed crystal.

13. The method for producing a gallium nitride crystal of claim 1 , wherein a temperature inside the reactor in the growing of the gallium nitride crystal is from 500 to 650° C.

14. The method for producing a gallium nitride crystal of claim 1 , wherein the gallium nitride crystal is grown under a pressure of from 120 to 350 MPa.

15. The method for producing a gallium nitride crystal of claim 1 , wherein a temperature inside the reactor in the growing of the gallium nitride crystal is from 500 to 530° C.

16. The method for producing a gallium nitride crystal of claim 1 , wherein a temperature inside the reactor in the growing of the gallium nitride crystal is 500 to 515° C.

17. The method for producing a gallium nitride crystal of claim 1 , wherein the gallium nitride crystal is grown under a pressure of from 150 to 300 MPa.

18. The method for producing a gallium nitride crystal of claim 1 , wherein the starting material is gallium nitride.

Assignments (3)
CHANGE OF NAME Recorded Sep 5, 2017
From: MITSUBISHI RAYON CO., LTD.
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 043750/0834 →
MERGER Recorded Sep 4, 2017
From: MITSUBISHI CHEMICAL CORPORATION
To: MITSUBISHI RAYON CO., LTD.
Reel/Frame 043750/0207 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 15, 2012
From: FUJISAWA, HIDEO; MIKAWA, YUTAKA; KAMADA, KAZUNORI
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 028385/0324 →
Continuity (3)
Provisional Application 61466154 · Mar 22, 2011
Provisional Application 61513270 · Jul 29, 2011
Related Publication 20120251431A1 · Oct 4, 2012