Gallium purification device and method

A purification method and crystallization tank technology, applied in the field of gallium purification devices, can solve the problems of difficult to control the crystal growth direction, high-purity gallium pollution, difficult solid-liquid separation, etc., and achieve the effect of facilitating automatic control, changing the separation method, and avoiding pollution.

Active Publication Date: 2020-03-31
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The innovations of the above-mentioned existing crystallization methods for purification of the prior art mainly focus on temperature field control and the continuous use of multiple methods, but no attention has been paid to the separation of crystallization mother liquor and crystal gallium after crystallization and the control of crystal growth direction; and The existing crystallization process adopts crystallization from the bottom, the final gallium crystal is on the bottom, and the crystallization mother liquor is on the top
[0010] In addition, due to the unevenness of the crystallization surface and the crystallization mother liquor only accounting for about 15%, it is difficult to separate the solid from the liquid; at present, the method of gradually extracting the upper liquid with a spoon is used in production to realize the solid-liquid separation, and the liquid is separated and then heated and melted Crystal emits high-purity gallium from the bottom
The above-mentioned process and operation have the following problems: (1) The separation of crystalline gallium and the crystallization mother liquor is not complete; (2) The incompletely decomposed mother liquor will cause pollution of high-purity gallium due to the enrichment of a large amount of impurities; (3) The whole system is difficult to Realize mechanized control; (4) It is difficult to control the crystal growth direction, and there are problems such as entrainment, resulting in low purification efficiency

Method used

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Experimental program
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Effect test

Embodiment 1

[0045] After the gallium purification device is installed, 4N gallium is melted at 45°C to form crystallization mother liquor, and the crystallization mother liquor is fed into the crystallization tank through the feeding pipe. The angle θ formed between the upper part of the crystallization tank and the horizontal direction is 75 degrees, and the lower part of the crystallization tank The angle α formed with the horizontal direction is 30 degrees; the distance between the upper liquid level of the crystallization mother liquid in the crystallization tank and the crystallization slot is 18cm measured by the tray rod with scale; the temperature of the closed space in the upper part of the cover is controlled by the temperature controller The temperature is 50°C; start the rotating device to rotate the tray rod, so that the seed crystal plate slowly moves down 18cm so that the lower surface of the seed crystal touches the upper surface of the crystallization mother liquor; start t...

Embodiment 2

[0047] After the gallium purification device is installed, 4N gallium is melted at 70°C to form crystallization mother liquor, and the crystallization mother liquor is fed into the crystallization tank through the feeding pipe. The angle θ formed between the upper part of the crystallization tank and the horizontal direction is 30 degrees, and the lower part of the crystallization tank The angle α formed with the horizontal direction is 75 degrees; the distance between the upper liquid level of the crystallization mother liquid in the crystallization tank and the crystallization slot is 18cm measured by the tray rod with scale; the temperature of the closed space in the upper part of the cover is controlled by the temperature controller The temperature is 35°C; start the rotating device to rotate the tray rod, so that the seed crystal plate slowly moves down 18cm so that the lower surface of the seed crystal touches the upper surface of the crystallization mother liquor; start t...

Embodiment 3

[0049] After the gallium purification device is installed, 4N gallium is melted at 30°C to form a crystallization mother liquor, and the crystallization mother liquor is fed into the crystallization tank through the feeding pipe. The angle θ formed between the upper part of the crystallization tank and the horizontal direction is 45 degrees, and the lower part of the crystallization tank The angle α formed with the horizontal direction is 40 degrees; the distance between the upper liquid level of the crystallization mother liquid in the crystallization tank and the crystallization tank opening is 18cm measured by the tray rod with scale; the temperature of the closed space in the upper part of the cover is controlled by the temperature controller The temperature is 29°C; start the rotating device to rotate the tray rod, so that the seed crystal plate slowly moves down 18cm so that the lower surface of the seed crystal touches the upper surface of the crystallization mother liquo...

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Abstract

The invention relates to a gallium purification device and method. The gallium purification device comprises a cooling assembly, a seed crystal assembly and a crystallizing tank assembly. The crystallizing tank assembly is located under the seed crystal assembly and fixedly connected with the seed crystal assembly. The cooling assembly comprises a cooling fluid storage tank, a cooling jacket and aconnecting pipe for connecting the cooling fluid storage tank with the cooling jacket. The crystallizing tank assembly comprises a delivery pipe, a crystallizing tank, a discharge pipe and a diaphragm. The crystallizing tank comprises an crystallizing tank upper portion and a crystallizing tank lower portion. The diaphragm is located between the crystallizing tank upper portion and the crystallizing tank lower portion in a separation mode. The delivery pipe and the discharge pipe both communicate with the crystallizing tank. The included angle theta is formed between the crystallizing tank upper portion and the horizontal direction. The included angle alpha is formed between the crystallizing tank lower portion and the horizontal direction. The diameter of the horizontal cross section ofthe crystallizing tank upper portion gradually increases from top to bottom. The crystallizing tank upper portion is partially or totally wrapped by the cooling jacket. Through the gallium purification device and method, a temperature field can be provided. The gallium purification device conducts crystallization under the temperature field and can gradually move downwards from the upper surface of molten gallium in the gallium crystallization process.

Description

technical field [0001] The invention relates to the field of high-purity gallium preparation, in particular to a gallium purification device and method. Background technique [0002] High-purity gallium and its compounds are widely used in high-tech fields of modern equipment manufacturing such as petrochemical industry, solar photovoltaic system, national defense aerospace, signal image processing, and modern automobile industry. In addition, high-purity gallium is also widely used in electronic devices such as eutectic alloys, epitaxial wafers and optoelectronic devices. With the popularization of new concepts such as low-carbon economy and green energy, the application range of high-purity gallium in the above fields will expand, and the market demand for high-purity gallium will continue to increase. [0003] At present, the preparation methods of high-purity gallium mainly include crystallization, vacuum distillation, electrolytic refining, chemical extraction, thermal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B58/00C30B29/02C30B35/00
CPCC22B58/00C30B29/02C30B35/00
Inventor 田庆华秦红郭学益李栋许志鹏朱刘何志达
Owner CENT SOUTH UNIV
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