High-purity gallium crystallization device and method

Abstract

The invention provides a high-purity gallium crystallization device and method. The crystallization device comprises a crystallization pipe, a thermostatic waterbath, a thermostatic stirrer and a stirring control device; the thermostatic stirrer is arranged in a crystallization pipe, the temperature difference exists between the thermostatic stirrer and the thermostatic waterbath, and the crystallization pipe is arranged in the thermostatic waterbath; and the upper end of the thermostatic stirrer is provided with the stirring control device. The method for preparing high-purity gallium throughthe crystallization device comprises the steps that a molten metal gallium raw material is added into the crystallization pipe, the temperature of the thermostatic waterbath is controlled to be 20-29DEG C, the temperature of the thermostatic stirrer is controlled to be 30-40 DEG C, the thermostatic stirrer moves up and down and is controlled to move in a reciprocating mode by 2-20 times per minute, the crystallization time is controlled to be 4-12 h, solid-liquid separation is conducted, and solid gallium is obtained; and the step is repeated by 3-5 times, and the high-purity gallium with the purity being 99.9999-99.999999% is obtained. The device is simple in operation method, and the obtained gallium is high in purity and good in reproducibility.

Description

technical field [0001] The invention relates to the technical field of high-purity gallium production, in particular to a high-purity gallium crystallization device and method. Background technique [0002] Gallium 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; according to product uses, "6N" gallium is mainly used for doped GaAs, GaP, GaSb and other semiconductor materials, not only requiring the purity of the product to reach 99.9999%. Especially for the content of Si, Fe, Zn, Cu and other elements, the requirements are strict. "7N" gallium is mainly used to make semi-insulating gallium arsenide for IC substrates. Except for C, N, O and Ta, the content of main impurities must be below 0.005ppm, which is generally called circuit-grade ultra-pure gallium. For gallium used as MBE source, the content of all impurity elements except C, N, O and Ta sho...

AI Technical Summary

Problems solved by technology

Due to the uncertain movement track, especially the non-straight-line reciprocating motion during the descent, it is easy to hit the crystallization tank repeatedly, and as the crystal height of the crystallization tank increases, it is very easy to cause the stirring rod and the bottom of the crystallization tank to break

[0004] Presently published patent applications such as the crystallization devices described in CN10487822A and CN203256317U are complicated and costly. The crystallization method described in patent application CN101386923A has a slow crystallization rate and a small amount of crystallization and cannot be produced in large quantities. The crystallization method described in patent application CN106048262A has temperature distribution Inhomogeneity, unstable solid-liquid interface, difficult solid-liquid separation, etc.

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