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A kind of production equipment and method of high-purity gallium

A production method and high-purity technology, applied in the field of high-purity gallium production equipment, can solve the problems of insufficient heat exchange between the medium and gallium liquid, the inability to effectively control the crystallization solidification rate, and difficulty in forming and agglomerating impurities, achieving good application prospects , Improve heat exchange efficiency and shorten production cycle

Active Publication Date: 2022-05-13
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technologies and inventions that have been disclosed so far provide many methods for preparing high-purity gallium by crystallization, but there are some shortcomings in the existing crystallization technology: 1. After each crystallization, the liquid gallium on the surface is sucked out with a straw or by some means Pour out, which is not conducive to simplifying the operation process, such as patent CN106636682B
2. The process of placing the seed crystal is complicated, and some methods even need to pour out the gallium liquid when adding the seed crystal for the second time, which is inconvenient for continuous production, such as patent CN104878224B and patent application CN101082086A
3. The solidification rate of each crystallization cannot be effectively controlled. It can only be realized by observing or estimating the crystallization time and discharging the residual gallium in time, which is not conducive to industrial production, such as patent CN106048262A
4. The heat exchange between the medium and the gallium liquid is not good enough, resulting in crystallization without orientation, and the impurities in the gallium liquid are difficult to form a good aggregation, such as patent CN104878224B

Method used

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  • A kind of production equipment and method of high-purity gallium
  • A kind of production equipment and method of high-purity gallium
  • A kind of production equipment and method of high-purity gallium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A high-purity gallium production equipment, such as figure 1 As shown, it includes a crystallization tank 1, a medium circulation tank, a thermal insulation layer 7 and a liquid gallium discharge device; the upper left side of the crystallization tank 1 is provided with a crystallization tank inlet 3, and the upper right side is provided with a crystallization tank outlet 4; the medium circulation tank It includes n independent medium circulation tanks, where n is an integer, 5≤n≤10; each medium circulation tank is composed of a circulation body, a medium inlet and a medium outlet, and the n medium circulation tanks are sequentially arranged from left to right Distributed laterally along the crystallization tank 1, the circulation body of each medium circulation tank is located inside the crystallization tank 1, and the medium inlet and medium outlet extend through the crystallization tank 1 to the outside of the crystallization tank 1; the heat insulation layer 7 is dis...

Embodiment 2

[0034] Such as figure 2 As shown, the difference between the device of this embodiment and Embodiment 1 lies in: (1) n is 7.

[0035] Compared with Example 1, the production steps of this embodiment differ in that: (1) both the cold medium and the heat medium are ethylene glycol; (2) the flow rate of the cold medium is 10 L / h, and the medium temperature is 2°C; (3) The heat medium flow rate of the first medium circulation tank 201-the sixth medium circulation tank 206 is 10L / h, and the medium temperature is 35°C; (4) The heat medium flow rate of the seventh medium circulation tank 207 is 10L / h, and the medium temperature (5) Step 6, repeat steps 2 to 5 5 times, so that the gallium in the crystallization tank 1 is crystallized again 5 times.

[0036] Table 3 is the impurity content table of the high-purity gallium prepared in this embodiment. The impurity elements above the detection limit in the high-purity gallium prepared by the method of the present invention include Cu ...

Embodiment 3

[0041] Such as Figure 3-Figure 4 As shown, the difference between the device of this embodiment and Embodiment 1 is: (1) n is 5; (2) the shape of the crystallization tank 1 is a cuboid, and (3) the circulation main body of each medium circulation tank is in a row shape.

[0042] Compared with Example 1, the production steps of this embodiment differ in that: (1) both the cold medium and the heat medium are ethylene glycol; (2) the flow rate of the cold medium is 10L / h, and the medium temperature is 25°C; (3) The heat medium flow rate of the first medium circulation tank 201-the fourth medium circulation tank 204 is 10L / h, and the medium temperature is 80°C; (4) The heat medium flow rate of the fifth medium circulation tank 205 is 10L / h, and the medium temperature 80°C; (5) Step 6, repeat steps 2 to 5 6 times, so that the gallium in the crystallization tank 1 is crystallized again 6 times; (6) The protective gas is high-purity argon.

[0043] Table 4 is the impurity content t...

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Abstract

The invention provides a high-purity gallium production equipment and method, including a crystallization tank, a medium circulation tank, a heat insulation layer and a liquid gallium discharge device. The method is: put circulating hot water into the medium circulation tank, place the processed liquid crude gallium in the crystallization tank through the entrance of the crystallization tank, feed circulating cold water into the first medium circulation tank, and pass through the crystallization tank after reaching the critical crystallization temperature. The seed crystal is placed at the entrance, and after each period of crystallization, the circulating cold water is passed into the next medium circulation tank until the penultimate medium circulation tank is filled with circulating cold water. After sufficient crystallization, the residual gallium liquid is discharged through the liquid gallium discharge device. Repeat the crystallization 5‑7 times, and the purity of the final product can reach 6‑7N. The equipment has simple structure, easy operation, environmental protection and energy saving, effectively shortens the production cycle, saves production costs and improves production efficiency.

Description

technical field [0001] The invention relates to the field of preparation of high-purity gallium, in particular to a production equipment and method of high-purity gallium. Background technique [0002] High-purity gallium is a key basic material for the preparation of semiconductor compounds. These semiconductor compounds are widely used in semiconductor industry and photovoltaic industry, etc. China is the world's largest producer of gallium, supplying more than 70% of global demand. Due to the high impurity content of coarse gallium, its application is limited and its added value is low. In order to increase the added value of gallium and expand its application range, the industry uses crude gallium as a raw material to prepare high-purity gallium (above 6N) through different purification methods. At present, the technologies for preparing high-purity gallium can be mainly divided into two categories: indirect purification method and direct purification method. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B58/00C22B9/02
CPCC22B58/00C22B9/02C22B9/006Y02P10/20
Inventor 王友彬洪标韦悦周袁增崟林学亮邹睿
Owner GUANGXI UNIV