Manufacturing method and manufacturing apparatus of a group III nitride crystal, utilizing a melt containing a group III metal, an alkali metal, and nitrogen

Patent metadata

Field	Value
Publication number	US-9376763-B2
Application number	US-201213679499-A
Country	US
Kind code	B2
Filing date	Nov 16, 2012
Priority date	Mar 14, 2005
Publication date	Jun 28, 2016
Grant date	Jun 28, 2016

Abstract

A method for manufacturing a group III nitride crystal on a seed crystal in a holding vessel holding therein a melt containing a group III metal, an alkali metal and nitrogen. The manufacturing method comprises the steps of causing the seed crystal to make a contact with the melt, setting an environment of the seed crystal to a first state offset from a crystal growth condition while in a state in which said seed crystal is in contact with the melt, increasing a nitrogen concentration in the melt, and setting the environment of the seed crystal to a second state suitable for crystal growth when the nitrogen concentration of the melt has reached a concentration suitable for growing the seed crystal.

First claim

The invention claimed is:

1. A method for manufacturing a group III nitride crystal in a holding vessel holding a melt containing a group III metal, an alkali meta and nitrogen, comprising the steps of:
raising a temperature of said melt from room temperature to a crystal growth temperature:
dissolving nitrogen into said melt at the crystal growth temperature and a crystal growth pressure:
increasing a nitrogen concentration to a concentration level at which nucleation takes place to produce junk crystals:
contacting a seed crystal with said melt when a nitrogen concentration in said melt is stabilized as a result of the nucleation; and
growing the group III nitride crystal onto said seed crystal.

2. The method for manufacturing a group III nitride crystal as claimed in claim 1 , further comprising the step of removing microcrystals grown from a nucleus from said melt before causing said seed crystal to contact with said melt.

3. The method for manufacturing a group III nitride crystal as claimed in claim 1 , wherein said removing step comprises the steps of:
submerging said holding vessel in a fixed auxiliary vessel filled with said melt; and
pulling up said holding vessel for said fixed auxiliary vessel when said nitrogen concentration in said melt is stabilized, wherein said step of causing said seed crystal to make contact with said melt is conducted such that said seed crystal is contacted to said melt in said pulled up holding vessel.

4. The method for manufacturing a group III nitride crystal as claimed in claim 2 , wherein said step of removing comprises the step of:
inserting a movable auxiliary vessel filled with said melt into said holding vessel; and taking out said movable auxiliary vessel from said holding vessel after transferring said melt in said movable auxillary vessel to said holding vessel when said nitrogen concentration in said melt is stabilized.

5. The method for manufacturing a group III nitride crystal as claimed in claim 2 , wherein said removing step comprises the step of removing microcrystals precipitated on an inner wall surface of said holding vessel, and wherein said step of causing said crystal to make contact with said melt comprises the step of causing said seed crystal to said melt in said holding vessel after said microcrystals are removed.

6. The method for manufacturing a group III nitride crystal as claimed in claim 1 , further comprising the step of disposing a crystal growth blocking part blocking growth of microcrystals grown from said nuclei in a close proximity to an inner wall surface of said holding vessel, before causing said seed crystal to contact with said melt.

Assignees

• Iwata Hirokazu
• Sarayama Seiji
• Fukuda Minoru
• Takahashi Tetsuya
• Takahashi Akira
• Ricoh Co Ltd

Inventors

• Iwata Hirokazu
• Sarayama Seiji
• Fukuda Minoru
• Takahashi Tetsuya
• Takahashi Akira

Classifications

• C30B29/403

  AIII-nitrides · CPC title

• C30B9/00 Primary

  Single-crystal growth from melt solutions using molten solvents (by normal or gradient freezing C30B11/00; by zone-melting C30B13/00; by crystal pulling C30B15/00; on immersed seed crystal C30B17/00; by liquid phase epitaxial growth C30B19/00; under a protective fluid C30B27/00) · CPC title

• C30B17/00

  Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method (C30B15/00 takes precedence) · CPC title

• C30B29/406

  Gallium nitride · CPC title

• Y10T117/1024

  for crystallization from liquid or supercritical state · CPC title