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A device and method for preparing high-purity gallium

A high-purity, seeded technology, which is applied to the preparation equipment and field of high-purity gallium, can solve the problems of inconvenient separation of residual liquid gallium, unfavorable operation process, and lower production costs, achieve good application prospects, and improve crystallization and melting speed. , the effect of easy operation

Active Publication Date: 2017-02-22
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technologies and inventions disclosed at present provide a lot of beneficial information for preparing high-purity gallium by crystallization, but the following problems still exist in the existing crystallization technology: 1. After the liquid gallium reaches the solidification ratio, it is inconvenient to separate the residual liquid gallium. Every time it is sucked out with a straw or poured out by some means, it is not conducive to simplifying the operation process, such as patent CN101082086A; 2. The purification process needs to be carried out in a clean room or a vacuum glove box, which is not conducive to reducing production costs, such as patent CN101082086A and patent CN1287575A

Method used

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  • A device and method for preparing high-purity gallium
  • A device and method for preparing high-purity gallium
  • A device and method for preparing high-purity gallium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A device for preparing high-purity gallium, comprising an inner tank 1, an outer tank 2 and a cover 3, both of which are columnar or platform-shaped, and can be cylinders, prisms, circular frustums or prisms; the bottom of the inner tank 1 is provided with drainage The tube 6 and the drainage tube 6 are provided with a switch 7, and the inner wall of the liner 1 is provided with tubular seed crystal addition holes 8, the seed crystal addition holes 8 are evenly distributed on the inner wall of the liner, and the upper edge of the liner 1 is evenly distributed with bands. Threaded inner tank through hole 15; the side wall of the outer tank 2 is provided with a water inlet and 4 water outlets 5, and the bottom of the outer tank 2 is provided with a drainage tube piercing hole 12, and the inner side of the bottom of the outer tank 2 is evenly distributed for supporting the inner tank. The support column 11 of the liner 1; the cover 3 is provided with a protective gas inlet ...

Embodiment 2

[0061] The structure of the device for preparing high-purity gallium is the same as in Example 1, the difference is that:

[0062] 1. The wall thickness of the polytetrafluoroethylene liner is 1.3mm;

[0063] 2. The ratio of the volume of the cavity between the inner and outer tanks to the volume of the inner tank is 0.5:1.

[0064] Method is with embodiment 1, and difference is:

[0065] (1) The protective gas in the device is high-purity argon;

[0066] (2) the purity of grafted seed crystals is 6N;

[0067] (3) When the solidification rate of gallium in the device reaches 95%, open the switch on the residual gallium drainage tube to make the remaining liquid gallium flow out;

[0068] (4) Steps 4 and 5 were repeated until the gallium in the device was recrystallized 8 times, and 6N high-purity gallium was prepared in the device.

[0069] The yield of 6N high-purity gallium prepared by the method is 67%.

Embodiment 3

[0071] The structure of the device for preparing high-purity gallium is the same as in Example 1, the difference is that:

[0072] 1. The inner liner 1 and the outer liner 2 are sealed and connected by thread at the upper edge of the two, and at the drainage tube 6 and the drainage tube exit hole 12;

[0073] 2. The cover 3 is fixed on the top of the device by snapping on the upper edge of the liner 1;

[0074] 3. The ratio of the volume of the cavity between the inner and outer tanks to the volume of the inner tank is 0.6:1.

[0075] Method is with embodiment 1, and difference is:

[0076] (1) The temperature of the cooling water is 20°C;

[0077] (2) the purity of grafted seed crystals is 6N;

[0078] (3) When the solidification rate of gallium in the device reaches 95%, open the switch on the residual gallium drainage tube to make the remaining liquid gallium flow out;

[0079] (4) Steps 4 and 5 were repeated until the gallium in the device was recrystallized seven time...

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Abstract

The invention provides a device and a method for preparing high-purity gallium, aims at the problems of the existing high-purity gallium preparation technology and belongs to the fields of the preparation equipment and the preparation technology of the high-purity gallium. The device comprises an inner container, an outer container and a cover; the inner container is located inside the outer container; a cavity for cold water and hot water to circulate alternately is arranged between the inner container and the outer container; the drainage tube of the inner container extends out of the outer container via the drainage tube passing hole of the outer container; the inner container is hermetically connected with the outer container; the cover is fixed on the top of the device. The method comprises the following steps: putting coarse gallium into the inner container, introducing cooling water into the cavity between the inner container and the outer container to crystallize the gallium, when the solidification rate of the gallium is within the range of 90-97%, discharging the left liquid gallium and then introducing hot water to melt the gallium, next, introducing the cooling water, and repeating crystallization for 6-8 times to improve the purity, thereby obtaining the high-purity gallium of 6N or 7N. The application method of the device is simple and convenient to operate; the obtained gallium is high in purity and high in yield, and has favorable application prospect.

Description

technical field [0001] The invention belongs to the field of high-purity gallium preparation equipment and preparation technology, and in particular relates to a device and method for preparing high-purity gallium. Background technique [0002] The existing preparation methods of high-purity gallium are mainly divided into two types: one is the indirect purification method, including: chemical extraction method, gallium trichloride method, metal organic compound synthesis method and microbial degradation method, etc., for example, patent CN103114214A discloses a A method for indirect production of high-purity gallium by using organic compound purification-thermal decomposition process. Patent US4666575 discloses a method for indirect production of high-purity gallium by adopting crude gallium-gallium trichloride-high-purity gallium process. In general, indirect purification The preparation process of the method is cumbersome and difficult to control, and the production scale...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B58/00
Inventor 厉英潘科峰
Owner NORTHEASTERN UNIV LIAONING
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