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Crystal production method using supercritical solvent, crystal growth apparatus, crystal, and device

A manufacturing method and supercritical technology, which are applied in the directions of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems of low growth crystal yield, high cost, easy heat escape, etc., and achieve the purpose of suppressing the usage amount and simplifying the structure. , the effect of reducing costs

Inactive Publication Date: 2008-07-02
MITSUBISHI CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the vicinity of the upper surface and the vicinity of the bottom of the autoclave 3 are different from the sides, and are not directly heated by an electric furnace, so heat is easy to escape and low temperature is easily formed.
In such a low-temperature portion, there is a problem that the crystallization raw material in a supersaturated state is not only on the seed crystal 10, but also in the form of precipitates on the holding member (not shown) for fixing the seed crystal and the inner wall of the autoclave 3. precipitation
[0009] However, the installation of the above-mentioned thermal insulation material and the improvement of the electric furnace will lead to an increase in the size and complexity of the crystallization device.
In addition, the installation of trapping nets and the like has the problem that the yield of grown crystals decreases due to precipitation outside the target crystal growth sites such as seed crystals.
It is possible to use a lining structure made of a corrosion-resistant material such as the above-mentioned noble metal in the main body of the autoclave to cope with this high corrosion, but it is very difficult to realize a lining structure such as a noble metal in the pipe and valve, and it is not preferable because of the high cost. of

Method used

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  • Crystal production method using supercritical solvent, crystal growth apparatus, crystal, and device
  • Crystal production method using supercritical solvent, crystal growth apparatus, crystal, and device
  • Crystal production method using supercritical solvent, crystal growth apparatus, crystal, and device

Examples

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Embodiment 1

[0163] Polycrystalline h-GaN (hexagonal gallium nitride) was used as a raw material, ammonia was used as a solvent, and helium gas was used as a substance (X), added to the autoclave, and crystal growth of gallium nitride was carried out by the following method. In addition, the critical densities of ammonia and helium are 0.234 g cm -3 , 0.0693g cm -3 , the density difference is 70.4%.

[0164] He added to the autoclave using the addition apparatus shown in FIG. 3 , and was implemented using the crystal production apparatus shown in FIG. 1 .

[0165] In an autoclave made of Inconel 625 (approximately 40 ml, cross-sectional area 2 cm 2 ) having a catheter with an inner volume of 2 ml lined with platinum (about 3% of the upper part including the lid, gasket, etc. is not lined with platinum). , 1.0g of polycrystalline h-GaN (hexagonal gallium nitride) was added as a raw material, and 0.2g of fully dried NH was added as a mineralizer. 4 Cl, then set the baffle plate and the cr...

Embodiment 2

[0169] Using polycrystalline h-GaN (hexagonal gallium nitride) and metal Ga as raw materials, and using ammonia as a solvent, crystal growth of gallium nitride was carried out by the following method. In addition, during crystal growth, the raw material metal Ga reacts with ammonia to generate hydrogen gas in the autoclave. The critical densities of ammonia and hydrogen are 0.234 g cm -3 , 0.03102g cm -3 , the density difference is 86.7%.

[0170] An autoclave made of Inconel 625 was used in the same autoclave as in Example 1, which had a catheter with an inner volume of 2 ml and was lined with platinum (about 3% of the upper part including the lid, gasket, etc. was not lined with platinum). Kettle (about 40ml, cross-sectional area 2cm 2 ), 1.0 g of raw polycrystalline h-GaN (hexagonal gallium nitride) and 1.0 g of metallic Ga were added, and 0.4 g of fully dried NH was added as a mineralizer. 4 After Cl, a baffle plate and a crystal growth part such as a seed crystal were...

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Abstract

The purpose of the present invention is to have a predetermined amount of substances different from the critical density of the solvent in the reaction vessel, and carry out crystal growth by solvothermal method, thereby controlling the precipitation position of the crystal, improving the yield of the crystal, and preventing the crystal from being mixed with Impurities, so that the crystals are highly purified. The crystal production method of the present invention is to use a supercritical state and / or a subcritical state solvent and a raw material in a reaction vessel to grow crystals, and it is characterized in that, in the reaction vessel, there is For the substance (X) having a critical density difference of 25% or more, the precipitation position of crystals can be controlled by adjusting the amount of the substance (X).

Description

technical field [0001] The present invention relates to a method for producing crystals by a solvothermal method. In particular, it relates to a hydrothermal method (hydrothermal synthesis method) for crystal growth of crystal or zinc oxide (hereinafter, the chemical formula "ZnO" of zinc oxide is also used as a synonym) by using water as a solvent, or the use of ammonia or the like. Nitrogen solvent is used for the preparation of nitrides of periodic table Group 13 elements (hereinafter referred to as "Group 13 elements") represented by gallium nitride (hereinafter, the chemical formula "GaN" of gallium nitride is also used as a synonym), etc. A method for producing high-quality bulk crystals by an ammonothermal method for crystal growth, and a crystal producing apparatus. Background technique [0002] The solvothermal method is a general term for a method for producing crystals using a supercritical solvent, and is referred to as a hydrothermal method (hydrothermal synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/10C30B29/16C30B29/18C30B29/38
CPCC30B7/10C30B29/18C30B29/406Y10T117/1004C30B29/16C30B29/38
Inventor 川端绅一郎吉川彰镜谷勇二福田承生
Owner MITSUBISHI CHEM CORP
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