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Preparation method of high-purity gallium

A high-purity and pure technology, applied in the field of preparation of inorganic semiconductor material raw materials, can solve the problems of dendrite bridging, crystal easily broken, affecting the grade of metal gallium, etc., to achieve the effect of increasing the solidification rate, large cooling area and reducing the number of purification times.

Inactive Publication Date: 2007-12-05
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, partial crystallization is used to prepare ultra-high-purity Ga in the process of solidifying a cylindrical container, that is, solidifying from the inner wall of the container toward the center of the container or gradually solidifying from the bottom of the cylindrical container to the upper part. It is easy to produce dendrite bridging and other phenomena. Stirring is required during the solidification process. At a certain stirring speed, the fine particles will agglomerate into larger particles while growing up, and the crystals are easy to break when the stirring speed is too high. Become fine particles, affecting the grade of metal gallium

Method used

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preparation example Construction

[0019] The invention provides a method for preparing high-purity gallium, comprising the following steps:

[0020] A. The clean and dry hemispherical reaction vessel is heated with a water bath at a temperature of 15°C to 25°C, and 5-10g of liquid high-purity gallium is evenly coated on the inner surface of the hemispherical reaction vessel to form a seed crystal, and the molten Thick gallium is added into the hemispherical reaction vessel, and the solidification speed of gallium is controlled to be 0.5cm 3 / min~1.5cm 3 / min, when the solidified gallium accounts for 60% to 90% of the total amount, the liquid gallium is poured out;

[0021] B. The solid gallium obtained in step A is used as a raw material, and step A is repeated;

[0022] Repeat steps A and B three to five times to obtain high-purity gallium as a product.

[0023] The diameter of the hemispherical reaction vessel is 50mm-120mm, the hemispherical part of the hemispherical reaction vessel needs to be completel...

Embodiment 1

[0026] A hemispherical reaction vessel with a diameter of 50 mm is washed with electronic grade deionized water and then dried; the vessel is placed in a water bath at 25°C, the hemispherical part is completely submerged in the water, and 5g of liquid high-purity gallium with a purity of 6N is coated on the inner surface of the vessel , after the seed crystal is formed, add molten crude gallium with a temperature of 30°C and a purity of 4N, adjust the temperature of the water bath to control the solidification speed of Ga to 0.8cm 3 / min, when the solidification amount reaches 80%, pour out the unsolidified liquid Ga, and use the obtained solid Ga as a raw material, repeat the above process 3 times, and obtain 6N high-purity gallium.

Embodiment 2

[0028] A hemispherical reaction vessel with a diameter of 80 mm is washed with electronic grade deionized water and then dried; the vessel is placed in a water bath at 24°C, the hemispherical part is completely submerged in the water, and 8 g of liquid high-purity gallium with a purity of 6N is coated on the inner surface of the vessel , after the seed crystal is formed, add molten gallium with a temperature of 30°C and a purity of 4N, adjust the temperature of the water bath to control the solidification speed of Ga to 0.6cm 3 / min, when the solidification amount reaches 80%, pour out the unsolidified liquid Ga, and use the obtained solid Ga as a raw material, repeat the above process 4 times, and obtain 6N high-purity gallium.

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Abstract

The present invention provides high purity gallium preparing process, which includes the following steps: 1. heating cleaned and dried semispherical reaction container in a water bath, coating high purity liquid gallium of 5-10 g serving as seed crystal to the inner surface of the reaction container, adding molten coarse gallium product into the reaction container, solidifying 60-90 % of gallium in the controlled rate of 0.5-1.5 cu cm / min, and pouring out liquid gallium; and 2. repeating the step 1 with the obtained solid gallium as material for 3-5 times to obtain high purity gallium.

Description

1. Technical field [0001] The invention relates to the preparation of inorganic semiconductor material raw materials, in particular to a preparation method of gallium (Ga). 2. Background technology [0002] Ga is a precious scattered metal with a wide range of applications. It can be used in low-melting point alloys, superconducting materials, and heat carriers in atomic reactors; gallium oxide is a multifunctional material. In addition to being used as chips for computer memory and magnetic bubble storage components, it is also widely used in hidden communications. , infrared radiation diode oscillators, ferromagnetic materials, photoelectric materials, fluorescent materials and other fields; gallium salts can be used as catalysts and used to prepare drugs for treating cancer and osteoporosis. However, the most important use of Ga is the binary compound formed by reacting with As, Sb, P and other elements, which is a very important semiconductor material. [0003] All sem...

Claims

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Application Information

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IPC IPC(8): C22B58/00C22B9/16
Inventor 方峰蒋建清邵起越董岩涂益友王东静
Owner SOUTHEAST UNIV
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