Static crystallization device and preparation method of ultra-pure gallium
A technology of static crystallization and crystallization tank, which is applied in chemical instruments and methods, single crystal growth, crystal growth, etc. It can solve the problems of poor temperature reliability, high requirements for crystallization temperature control, and difficulty in ensuring high temperature uniformity in the crystallization device, etc. question
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[0042] The present invention also provides a method for preparing ultra-high-purity gallium, comprising the following steps:
[0043] The seed crystal is placed on the seed crystal seat of the crystallization device, and the raw gallium melt is poured into the crystallization tank for crystallization to obtain ultra-high-purity gallium;
[0044] The crystallization device is the static crystallization device described above.
[0045] In the present invention, the raw gallium is preferably preheated to 35-37°C in a clean, anhydrous and oxygen-free oven, kept at a constant temperature for 8-15 hours, and then put into the crystallization tank, which can ensure the initial The temperature is uniform to avoid the formation of gallium crystal nuclei in a certain part.
[0046] In the present invention, the temperature of the surface of the gallium melt is preferably 29-32°C, more preferably 29.5-30.5°C, most preferably 30°C; controlling the surface temperature of the gallium melt ...
Embodiment 1
[0055] according to figure 1 Install the crystallization purification device, install the seed crystal seat (the internal seed crystal is 7N gallium), ensure that the seed crystal is at 24.5-26°C, and the temperature of the cooling circulating water tank is between 27-29.5°C for more than 4H, and then pour into the crystallization tank Add the initial gallium melt (purity 6N) that has been preheated in advance.
[0056] During the crystallization process, the temperature of the seed crystal is controlled to be 25±0.2°C, the temperature of the cooling circulating water tank is 27.5±0.2°C, and the temperature of the surface of the gallium melt is 30±0.5°C. After 120 hours of crystallization, the upper gallium tail liquid was scooped out, and the volume of gallium crystals was measured to be about 91.3% by weighing. Table 1 shows the steps of impurities.
Embodiment 2
[0058] according to figure 1 Install the crystallization purification device, install the seed crystal seat (the internal seed crystal is 7N gallium), ensure that the seed crystal is at 24.5-26°C, and the temperature of the cooling circulating water tank is between 27-29.5°C for more than 4H, and then pour into the crystallization tank Add the initial gallium melt (purity 6N) that has been preheated in advance.
[0059] During the crystallization process, the temperature of the seed crystal is controlled to be 25±0.2°C, the temperature of the cooling circulating water tank is 28±0.2°C, and the temperature of the surface of the gallium melt is 30±0.5°C. After 120 hours of crystallization, the upper gallium tail liquid was scooped out, and the volume of gallium crystals was measured to be about 86.7% by weighing. Table 1 shows the steps of impurities.
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