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Method for preparing gallium nitride crystal by solid-state displacement reaction

A substitution reaction, gallium nitride technology, applied in chemical instruments and methods, self-solids, crystal growth, etc., can solve the problems of difficult large-scale industrial production, harsh growth conditions, and low crystal growth rate, and achieves easy promotion and growth. The effect of large-scale production, high crystal growth rate, and short synthesis time

Inactive Publication Date: 2010-12-15
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to overcome the shortcomings and deficiencies of the prior art, and provide a new method for preparing gallium nitride crystals, so as to solve the problems of low crystal growth rate and growth condition requirements in the preparation methods of gallium nitride crystals in the prior art. Harsh, high production cost, high energy consumption, difficult to large-scale industrial production and other issues

Method used

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  • Method for preparing gallium nitride crystal by solid-state displacement reaction
  • Method for preparing gallium nitride crystal by solid-state displacement reaction

Examples

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Effect test

Embodiment 1

[0023] Example 1: Take tetragonal lithium gallate and hexagonal boron nitride pellets with a molar ratio of 1:1, put them into a three-dimensional mixer, mix for about 30 minutes, and press the mixture into a cylindrical block with a mold. Put the pressed cylindrical block into the graphite tube of the pyrophyllite assembly block, and assemble the graphite sheet, molybdenum sheet and conductive steel ring at the upper and lower ends of the graphite tube in sequence. After assembly, place the high-pressure synthetic block in a large-cavity press at a temperature of about 850°C and a pressure of about 1.1GPa. After about 1 minute of heat preservation and pressure holding, the synthetic material is taken out after pressure relief and cooling, and the mass concentration is about Soak in 20% hydrochloric acid to wash out LiBO 2 After waiting for impurities, gallium nitride crystals are obtained.

Embodiment 2

[0024] Example 2: Take tetragonal lithium gallate and hexagonal boron nitride pellets with a molar ratio of 1:0.9, put them into a three-dimensional mixer, mix for about 45 minutes, and press the mixture into a cylindrical block with a mold. Put the pressed cylindrical block into the graphite tube of the pyrophyllite assembly block, and assemble the graphite sheet, molybdenum sheet and conductive steel ring at the upper and lower ends of the graphite tube in sequence. After assembly, place the high-pressure synthetic block in a large-cavity press at a temperature of about 1600°C and a pressure of about 5.0GPa. After about 20 minutes of heat preservation and pressure holding, the synthetic material is taken out after pressure relief and cooling, and the mass concentration is about Soak in 50% nitric acid to wash out LiBO 2 After waiting for impurities, gallium nitride crystals are obtained.

Embodiment 3

[0026] Take hexagonal lithium gallate and hexagonal boron nitride pellets with a molar ratio of 1:0.8, put them into a three-dimensional mixer, mix for about 40 minutes, press the mixture into a cylindrical block with a mold, and put the pressed The cylinder blocks are put into the graphite tube of the pyrophyllite assembly block, and the upper and lower ends of the graphite tube are sequentially assembled with graphite sheets, molybdenum sheets and conductive steel rings. After assembling, place the high-pressure synthetic block in a large-cavity press at a temperature of about 1400°C and a pressure of about 5.5GPa. After about 25 minutes of heat preservation and pressure holding, the synthetic material is taken out after pressure relief and cooling, and the mass concentration is Soak in 30% hydrochloric acid to remove LiBO 2 After waiting for impurities, gallium nitride crystals are obtained.

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Abstract

The invention discloses a method for preparing a gallium nitride crystal by utilizing the solid-state displacement reaction. The method mainly comprises the following steps: (1) reaction precursors of gallic acid lithium and boron nitride are mixed and pre-pressed into a block, or pre-pressed into sheets respectively, and the sheets are alternately piled into a block; (2) a block reactant which are obtained by the pre-pressing after mixing or alternate piling is put in a high-pressure synthesis block; (3) the assembled high-pressure synthesis block is placed in a synthesis cavity of a large presser for the solid-state displacement reaction, the synthesis temperature is not less than 850 DEG C, the pressure is not less than 1.0GPa, and the synthesis time is not less than 1.0 minute; and (4) after the displacement reaction, the reactant is subjected to cooling and pressure relief, and the synthesis product is taken out and soaked in acid liquor to dissolve and remove LiBO2, and the gallium nitride crystal is obtained. The method has the advantages of low raw material cost, low requirement on production specification, convenient operation, high growth rate of crystal, short synthesistime, easy popularization, mass production and the like.

Description

technical field [0001] The invention relates to a method for preparing gallium nitride crystals, in particular to a method for preparing gallium nitride crystals by solid-state replacement reaction. technical background [0002] Gallium nitride (GaN) is a wide bandgap compound semiconductor material with a room temperature bandgap of 3.4ev and good chemical and thermal stability. ) ideal material. This type of light source has wide application value and huge economic benefits in many aspects such as optical information storage, optical display, and optical illumination. [0003] Because GaN will decompose at 900°C under normal pressure, traditional crystal growth methods (such as: pulling method) cannot be applied to the preparation of GaN crystals. Among the main methods for preparing GaN in the prior art, the more successful methods include high-pressure solution growth (Porowski, S.J.Cryst.Growth 1996, 166, 583.), cosolvent method (Wang, B.et al.J.Cryst. Growth, 2006, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J3/06C30B29/38C30B1/10C30B29/40
Inventor 雷力贺端威
Owner SICHUAN UNIV
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