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Method for producing nitride crystals, and production vessel and members

A manufacturing method and nitride technology, applied in the field of ammonothermal method, can solve problems such as hindering crystal growth and lowering productivity, and achieve the effect of improving production efficiency and high quality

Active Publication Date: 2012-09-26
MITSUBISHI RAYON CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Gallium nitride microcrystals caused by the above-mentioned spontaneous crystal nuclei hinder the growth of crystals on the seed crystals that should have been precipitated, and cause a decrease in productivity.

Method used

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  • Method for producing nitride crystals, and production vessel and members
  • Method for producing nitride crystals, and production vessel and members
  • Method for producing nitride crystals, and production vessel and members

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0160] In this example, use figure 1 In the shown reaction device, the seed crystal and the test piece are suspended, and the experiment of heating the raw material is carried out.

[0161] An autoclave 1 made of Inconel 625 with a platinum-lined inner size of 15 mm in diameter and 154 mm in length (inner volume of about 27 cm 3 ),conduct experiment. The inner surface 2 of the autoclave 1 is thoroughly cleaned and dried. Similarly, platinum wires, platinum growth frames 6 , platinum baffles 5 , and platinum mesh raw material baskets used to support the test pieces were washed and dried.

[0162] Polycrystalline GaN particles were used as raw material 8 for nitride crystal growth. The polycrystalline GaN particles were washed with hydrofluoric acid at a concentration of about 50% by weight for the purpose of removing deposits, rinsed sufficiently with pure water, dried, and weighed 12.98 g into a raw material basket made of platinum mesh.

[0163] Weigh 0.74 g of fully drie...

Embodiment 2）

[0194] In Example 2, a bulk Ta-2.5% by weight W alloy was used as a test piece. The experiment was carried out under the same conditions as in Example 1 except that the point where the seed crystal was not attached was changed.

[0195] As a result of observing the appearance of the test piece after implementation of Example 2, there was almost no change from before implementation, and no deposits were observed. In the measurement by EPMA, the formation of GaN was not found on the surface. As a result of observing the unevenness of the test piece by a cross-sectional SEM, almost no unevenness was found.

[0196] The surface roughness of the same test piece as that of Example 2 was measured before the suspension test, and the surface roughness (Ra) was 0.463 μm. As a result of observing the cross section by EPMA, no nitride layer or other deteriorated layer was found on the surface of the test piece, and no corrosion was confirmed.

Embodiment 3）

[0198] In Example 3, plate-shaped tantalum was used as a test piece. The experiment was carried out under the same conditions as in Example 1 except that the point where the seed crystal was not attached was changed.

[0199] As a result of observing the appearance of the test piece after implementation of Example 3, there was almost no change from before implementation, and no deposits were observed. In the measurement by EPMA, the formation of GaN was not found on the surface. As a result of observation of irregularities of the test piece by cross-sectional SEM, it was confirmed that the cross section was extremely flat.

[0200] The surface roughness of the same test piece as that of Example 3 was measured before the suspension test, and the surface roughness (Ra) was 0.079 μm. As a result of observing the cross section by EPMA, no nitride layer or other deteriorated layer was found on the surface of the test piece, and no corrosion was confirmed.

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Abstract

Provided is a method for producing nitride crystals with which it is possible to inhibit precipitation of nitride crystals in parts other than on seed crystals and improve the efficiency of producing gallium nitride single crystals grown on seed crystals. When nitride crystals are produced by the ammonothermal method in a vessel holding a solution containing a mineralizer, the portions of the surfaces of the vessel and the members inside the vessel in contact with the solution are at least partially formed from a metal or alloy including one or more atoms selected from the group comprising tantalum (Ta), tungsten (W), and titanium (Ti), and the surface roughness (Ra) is less than 1.80 [mu]m.

Description

technical field [0001] The present invention relates to an ammonothermal method for growing nitride crystals. In particular, it relates to an ammonothermal method in which the material of the container for nitride crystal growth is characterized. Background technique [0002] The ammonothermal method is a method of producing a desired material by using an ammonia solvent in a supercritical state and / or a subcritical state and utilizing a dissolution-precipitation reaction of a raw material. When the ammonothermal method is used for crystal growth, the temperature dependence of the solubility of the raw material in the ammonia solvent is utilized, and a supersaturated state is generated by a temperature difference to precipitate crystals. [0003] The hydrothermal method, which is similar to the ammonothermal method, uses supercritical and / or subcritical water in a solvent for crystal growth, and is mainly used in crystal (SiO 2 ) and methods for crystallizing oxides such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/38C30B7/10
CPCC30B7/105C30B29/403C30B29/406C30B29/38C30B7/10Y10T117/1024Y10T117/102Y10T117/1096Y10T117/10
Inventor 三川丰清见真纪子镜谷勇二石黑彻山村美彦
Owner MITSUBISHI RAYON CO LTD
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