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A kind of Czochralski reuse method of gallium arsenide crystal residue

A gallium arsenide and crystal technology, which is applied in the field of compound semiconductor material reuse, can solve the problems of stoichiometric ratio deviation, interference with crystal growth, and difficulty in growing single crystals, etc., to achieve reduced impurity concentration, short time, and improved stoichiometric ratio Effect

Active Publication Date: 2016-06-01
GRINM GUOJINGHUI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These gallium arsenide crystal residues cannot be directly put into the single crystal production process according to the existing process technology, because if they are directly put into the single crystal growth process, the surface of the melt will be covered with gallium oxides, and the stoichiometric ratio Deviation, which seriously interferes with crystal growth and makes it difficult to grow single crystals, thus causing a lot of waste of raw materials

Method used

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  • A kind of Czochralski reuse method of gallium arsenide crystal residue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Material preparation and furnace loading: smash 2.0Kg of gallium arsenide crystal residues after corrosion cleaning into small pieces, put them into a quartz crucible, and then put 300g of boron oxide covering agent to seal the furnace body.

[0024] 2. Vacuumize the furnace to make the furnace pressure less than 400Pa, and then fill the furnace with 1.0MPa high-purity nitrogen.

[0025] 3. Raise the temperature of the material: raise the temperature to 1400°C to melt the gallium arsenide crystal residue, and control the furnace pressure at about 1.8MPa. Rotate the seed rod at a rate of 2 rpm and the crucible rod in the opposite direction at a rate of 10 rpm.

[0026] 4. Cooling and seeding: Adjust the temperature so that the seed crystal contacts the melt. When the seed crystal and the melt are in stable contact for 30 minutes, start cooling and seeding. The cooling rate is controlled at 0.05-0.4°C / min. When the solid-liquid interface is seen When the solid phase g...

Embodiment 2

[0031] 1. Prepare materials and load the furnace: smash 4.0Kg of gallium arsenide crystal residue after corrosion cleaning into small pieces, put them into a quartz crucible, then put 700g of boron oxide covering agent, and seal the furnace body.

[0032] 2. Vacuum to make the furnace pressure less than 200Pa. , and then fill the furnace with high-purity nitrogen gas 1.5MPa.

[0033] 3. Raise the material: raise the temperature to 1520°C to melt the gallium arsenide crystal residue, and control the furnace pressure at about 2.3MPa. Rotate the seed rod at a rate of 6 rpm and turn the crucible rod in the opposite direction at a rate of 15 rpm.

[0034] 4. Cooling and seeding: Adjust the temperature so that the seed crystal contacts the melt. When the seed crystal and the melt are in stable contact for 30 minutes, start cooling and seeding. The cooling rate is controlled at 0.2-1.0°C / min. When the solid-liquid interface is seen When the solid phase grows, start to pull the crys...

Embodiment 3

[0039] 1. Prepare materials and load the furnace: smash the 3.0Kg gallium arsenide crystal residue after corrosion cleaning into small pieces, put them into a quartz crucible, then put 500g of boron oxide covering agent, and seal the furnace body.

[0040] 2. Vacuumize the furnace to make the furnace pressure less than 300Pa, and then fill the furnace with 1.2MPa high-purity nitrogen.

[0041] 3. Raise the temperature of the material: raise the temperature to 1480°C to melt the gallium arsenide crystal residue, and control the furnace pressure at about 2.0MPa. Rotate the seed rod at a rate of 5 rpm and turn the crucible rod in the opposite direction at a rate of 12 rpm.

[0042] 4. Cooling and seeding: adjust the temperature so that the seed crystal contacts the melt. When the seed crystal and the melt are in stable contact for 30 minutes, start cooling and seeding. The cooling rate is controlled at 0.2-0.6 °C / min. When the solid-liquid interface is seen When the solid phase ...

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Abstract

The invention relates to a directly pulling reutilization method of a gallium arsenide crystal defective material. The method comprises the steps of preparing materials, loading the materials in a furnace, vacuumizing and filling gas, heating for melting the materials, cooling for inducing a crystal, isometric controlling, ending and unloading the materials. The method has the advantages that a chemical proportion of the gallium arsenide crystal defective material is greatly improved by drawing out the gallium arsenide crystal with a high-pressure liquid encapsulation pulling method, and at the same time, gallium oxides are all distributed on the surface of the gallium arsenide crystal and present protrusion shapes during the growth process of the crystal due to the density of the gallium oxides smaller than that of the gallium arsenide, so that 99% of the oxides can be removed by simple polishing with a grinding machine. By using the method to process the gallium arsenide crystal defective material, only 20 hours is needed for one period, without repeating processing problem. The method has high efficiency and simple operations, and the usually abandoned gallium arsenide crystal defective material can be reused for pulling the crystal, enabling the utilization rate of the gallium arsenide crystal defective material to reach over 95%.

Description

technical field [0001] The invention relates to a method for reusing compound semiconductor materials, in particular to a method for reusing Czochralski remnants of gallium arsenide crystals. Background technique [0002] Since gallium is easy to form an oxide film on the surface in the air, the gallium arsenide polycrystal synthesized by the horizontal gradient solidification method inevitably contains gallium oxide in the synthesized polycrystal; at the same time, the obtained polycrystal ingot is in the tail There is a gallium-rich part. In addition, the polycrystals synthesized by the horizontal gradient solidification method and the grown gallium arsenide single crystals, in the process of crystal synthesis or crystal pulling, due to frying furnace or gas leakage, will produce polycrystals with serious deviations in stoichiometric ratio and inclusion of more oxides. Crystal materials and gallium-rich materials. The above-mentioned gallium arsenide materials containing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/42C30B15/00C30B15/20
Inventor 林泉马英俊张洁李超郑安生
Owner GRINM GUOJINGHUI NEW MATERIALS CO LTD