# US 9,518,337 B2 · Method for producing nitride crystal and nitride crystal

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- Number: US 9,518,337 B2
- Document ID: US9518337B2
- Status: Granted
- Kind: B2
- Application number: 14/713,894
- Filed: 2015-05-15
- Published: 2015-09-03
- Granted: 2016-12-13
- Earliest claimed: 2011-10-28
- Assignees: Mitsubishi Chemical Corporation
- Applicants: Mitsubishi Chemical Corporation
- Inventors: Yutaka Mikawa; Hideo Fujisawa; Kazunori Kamada; Hirobumi Nagaoka; Shinichiro Kawabata; Yuji Kagamitani
- Web page: https://patentgrep.com/patent/US9518337B2

## CPC

- C30B 29/406: {Gallium nitride}
- C01B 21/0632: {with gallium, indium or thallium}
- C30B 7/105: {using ammonia as solvent, i.e. ammonothermal processes}
- C30B 29/403: {AIII-nitrides}
- H01S 5/3086: {doping of the active layer}
- H01S 5/32341: {blue laser based on GaN or GaP}
- H10D 62/605: {Planar doped, e.g. atomic-plane doped or delta-doped}
- H10D 62/8503: {Nitride Group III-V materials, e.g. AlN or GaN}
- H10D 62/854: further characterised by the dopants
- H10H 20/0137: {the light-emitting regions comprising nitride materials}
- H10H 20/8215: {characterised by crystalline imperfections, e.g. dislocations; characterised by the distribution of dopants, e.g. delta-doping}
- H10H 20/825: containing nitrogen, e.g. GaN
- H10H 20/8252: {characterised by the dopants}
- H10P 14/20: of semiconductor materials
- H10P 14/2908: {Nitrides}
- H10P 14/3416: {Nitrides}
- C01P 2004/50: Agglomerated particles
- C01P 2006/40: Electric properties
- C01P 2006/90: Other properties not specified above
- H01S 2304/00: Special growth methods for semiconductor lasers
- Y02P 20/54: using solvents, e.g. supercritical solvents or ionic liquids
- Y10T 428/2982: Particulate matter [e.g., sphere, flake, etc.]
- C30B: SINGLE-CRYSTAL GROWTH (by using ultra-high pressure, e.g. for the formation of diamonds, B01J3/06); UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL (zone-refining of metals or alloys C22B); PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (casting of metals, casting of other substances by the same processes or devices B22D; working of plastics B29; modifying the physical structure of metals or alloys C21D, C22F); SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE (for producing semiconductor devices or parts thereof H10); APPARATUS THEREFOR
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H01S: DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H10D: INORGANIC ELECTRIC SEMICONDUCTOR DEVICES
- H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS
- H10P: GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

A high-quality nitride crystal can be produced efficiently by charging a nitride crystal starting material that contains tertiary particles having a maximum diameter of from 1 to 120 mm and formed through aggregation of secondary particles having a maximum diameter of from 100 to 1000 μm, in the starting material charging region of a reactor, followed by crystal growth in the presence of a solvent in a supercritical state and/or a subcritical state in the reactor, wherein the nitride crystal starting material is charged in the starting material charging region in a bulk density of from 0.7 to 4.5 g/cm3 for the intended crystal growth.

## Claims

### Claim 1

A GaN starting material for producing a GaN crystal, comprising:
a material having an angle of repose and comprising a plurality of polycrystalline GaN particles having a maximum diameter of from 0.5 to 1 mm,
wherein the material has a bulk density of from 0.7 to 4.5 g/cm3.

### Claim 2 (depends on 1)

The GaN starting material according to claim 1, wherein the material comprises a plurality of particles formed through aggregation of the polycrystalline GaN particles having the maximum diameter of from 0.5 to 1 mm.

### Claim 3 (depends on 2)

The GaN starting material according to claim 2, wherein the particles formed through aggregation have a maximum diameter of not smaller than 1 mm.

### Claim 4 (depends on 1)

The GaN starting material according to claim 1, wherein the angle of repose is less than 45°.

### Claim 5 (depends on 1)

The GaN starting material according to claim 1, wherein the bulk density is from 0.8 to 3.6 g/cm3.

### Claim 6 (depends on 1)

The GaN starting material according to claim 1, wherein the material has an oxygen concentration in a crystal of from 10 to 500 ppm.

### Claim 7 (depends on 1)

The GaN starting material according to claim 1, wherein the bulk density is from 0.9 to 3.2 g/cm3.

### Claim 8 (depends on 1)

The GaN starting material according to claim 1, wherein the bulk density is from 1.0 to 3.0 g/cm3.

### Claim 9 (depends on 1)

The GaN starting material according to claim 1, wherein the bulk density is from 1.1 to 3.0 g/cm3.

### Claim 10 (depends on 1)

The GaN starting material according to claim 1, wherein the angle of repose is not smaller than 15°.

### Claim 11 (depends on 1)

The GaN starting material according to claim 1, wherein the angle of repose is not smaller than 25°.

### Claim 12

A method for producing a GaN crystal, comprising:
growing a GaN crystal in the presence of nitrogen in a supercritical state and/or a subcritical state and a GaN starting material which comprises a material having an angle of repose, having a bulk density of from 0.7 to 4.5 g/cm3 and comprising a plurality of polycrystalline GaN particles having a maximum diameter of from 0.5 to 1 mm.

### Claim 13 (depends on 12)

The method according to claim 12, wherein the material comprises a plurality of particles formed through aggregation of the polycrystalline GaN particles having the maximum diameter of from 0.5 to 1 mm.

### Claim 14 (depends on 12)

The method according to claim 12, wherein the particles formed through aggregation have a maximum diameter of not smaller than 1 mm.

### Claim 15 (depends on 12)

The method according to claim 12, wherein the angle of repose is less than 45°.

### Claim 16 (depends on 12)

The method according to claim 12, wherein the bulk density is from 0.8 to 3.6 g/cm3.

### Claim 17 (depends on 12)

The method according to claim 12, wherein the material has an oxygen concentration in a crystal of from 10 to 500 ppm.

### Claim 18 (depends on 12)

The method according to claim 12, wherein the bulk density is from 0.9 to 3.2 g/cm3.

### Claim 19 (depends on 12)

The method according to claim 12, wherein the bulk density is from 1.0 to 3.0 g/cm3.

### Claim 20 (depends on 12)

The method according to claim 12, wherein the bulk density is from 1.1 to 3.0 g/cm3.