Method and apparatus for preparing high-purity gallium

A high-purity, container technology, applied in the field of high-purity gallium preparation, can solve the problems of unstable crystal interface, many factors affecting quality, low purification efficiency, etc., to reduce the possibility of impurity introduction, good product stability, and improve purification. effect of effect

Active Publication Date: 2015-06-17
NORTHEASTERN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The general preparation process adopts a combination of multiple methods of purification, the process is relatively complicated, there are many factors affecting quality, and the product quality is not easy to control
For example, the electrolytic refining method requires strict environmental purity, the current efficiency of the electrolysis process is relatively low, the electrolysis time is long, the investment is large, the energy consumption is high, and the application is restricted.
Both the zone smelting method and the VGF method use the metal segregation phenomenon to realize the purification of metal gallium, but because gallium has a low melting point (29.78°C), the change of ambient temperature will have a great impact on the crystallization, and the solid-liquid interface is not easy. control, and the crystal interface is unstable, and the purification efficiency is low
[0004] The Chinese patent application announcement number CN103160856A published on June 19, 2013, "Preparation method of high-purity gallium", proposes a method combining electrolytic refining and crystallization. Although high-purity gallium can be obtained, the entire process is complicated and electrolytic The production cycle is long, the environmental factors are strict, and the production cost is high
[0005] The patent of Chinese Patent Application Publication No. CN1619018A published on May 25, 2005 proposes a method combining electrolysis and zone melting, but the process is long and the cost of equipment is high. high frequency power consumption
[0006] Chinese Patent Application Publication Nos. CN101413068A and CN101082086A disclose methods for preparing high-purity gallium that utilize the crystallization principle of metal gallium, but in the disclosed method, it is necessary to repeat the process of "crystallization of liquid gallium—the poured out part is crystalline liquid gallium—melting The operation process of crystallized gallium metal - pouring into the device for cooling" will increase the additional loss of metal gallium in the process, increase the work intensity of multiple operations, and increase the possibility of impurities being brought in

Method used

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  • Method and apparatus for preparing high-purity gallium

Examples

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Effect test

Embodiment 1

[0030] Such as figure 1 As shown, the method for preparing high-purity gallium is to first place liquid high-purity metal gallium at the bottom of the cooling container 2, and cool it as a seed crystal; pour liquid metal gallium into the cooling container, and apply a constant temperature cold source 5 at the bottom of the cooling container. , carry out cooling and crystallization; after the liquid metal gallium is completely crystallized and solidified, turn on the heat source coil 3 to make the coil move from the bottom to the top of the container, and control the temperature and moving speed of the coil through the control device 9 to maintain the solid-liquid interface during the solidification process Stable; repeat the heat source coil moving operation many times to achieve the purpose of purification, the crystallization interception rate is 70%-90%, and metal gallium above 6N can be obtained.

[0031] This device for preparing high-purity gallium includes a cooling con...

Embodiment 2

[0033] The device for preparing high-purity gallium is the same as in Example 1. A constant-temperature cold source is applied to the bottom of a cylindrical cooling container made of plexiglass. The temperature of the cold source is 3°C. The ethylene glycol refrigerant is provided to the cold end of the container through copper heat conduction. 5g of high-purity liquid gallium with a purity of 6N is coated on the bottom of the container to form a seed crystal, and liquid metal gallium with a purity of 4N is added at a temperature of 35°C. Move from bottom to top, control the temperature of the heat source coil at 40°C, the moving speed at 1cm / h, and the temperature of the bottom cold source at 3°C. After repeating the operation of moving the heat source coil 4 times, intercept 80% of gallium metal to obtain 6N high-purity gallium.

Embodiment 3

[0035] The device for preparing high-purity gallium is the same as in Example 1. A constant-temperature cold source is applied to the bottom of a cylindrical cooling container made of plexiglass. 5g of high-purity liquid gallium with a purity of 6N is coated on the bottom of the container to form a seed crystal, and liquid metal gallium with a purity of 4N is added at a temperature of 40°C. Move from bottom to top, control the temperature of the heat source coil at 50°C, the moving speed at 0.5cm / h, and the temperature of the bottom cold source at 0°C. After repeating the operation of moving the heat source coil 4 times, intercept 85% of the gallium metal to obtain a 6N high pure gallium.

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Abstract

The present invention discloses a method and an apparatus for preparing high-purity gallium. According to the method, liquid-state high-purity gallium is placed on the bottom portion of a container and is cooled as a seed crystal, the liquid-state metal gallium is poured into the cooling container to cool and crystallize, a thermal source coil is opened after complete crystallization, the temperature and the movement speed of the thermal source coil are controlled, the thermal source coil moves from bottom to top, the stable solid-liquid interface during the solidification process is ensured, the solidification interception ratio is 70-90%, and the metal gallium can be purified to achieve more than or equal to 6N. The apparatus comprises the cooling container, a constant temperature cold source, the thermal source coil and a control device, wherein the bottom portion of the cooling container is provided with the constant temperature cold source, the upper portion of the cooling container is provided with a dust preventing cover, the thermal source coil sleeves on the outer side of the cooling container, and the thermal source coil is connected with the control device through a conducting wire so as to make the temperature and the movement speed of the thermal source coil be controlled by the control device. According to the present invention, characteristics of simple apparatus mechanism, easy method operation, convenient specification quantifying, good product stability and the like are provided.

Description

technical field [0001] The invention relates to a method and device for purifying high-purity gallium, in particular to a preparation method and device for purifying 3N-4N gallium to ≥6N high-purity gallium, which belongs to the technical field of high-purity gallium preparation. Background technique [0002] Gallium (Ga) is a typical scattered metal, and it is one of the rare metals that are purchased and stored as a national strategy. As an important semiconductor basic material, high-purity gallium is widely used in the fields of electronic materials, optoelectronic materials, optical materials and thermoelectric materials. Gallium compound semiconductor materials (GaAs, GaN, GaP, GaAlAs, etc.) have become one of the important supporting materials in the fields of contemporary communications, integrated circuits, aerospace, energy and even medical care. The high-purification and refined preparation of gallium metal is an important way to develop high value-added products...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B58/00
Inventor 姜澜丁友东苏楠邱明放付高峰
Owner NORTHEASTERN UNIV
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