A kind of method for preparing high-purity silicon particles
A silicon particle, high-purity technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., to achieve the effect of strong controllability, high efficiency and few steps
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Embodiment 1
[0122] High-purity silicon particles were prepared as follows.
[0123] Obtain raw silicon granules: impact the raw silicon block (ferrosilicon block) into smaller raw silicon small blocks. Then, using a high-energy ball milling process, the above-mentioned raw silicon small pieces were ball-milled for 2 hours at a speed of 800 rpm in an argon atmosphere using a 3mm ball mill; and then used at a speed of 1100 rpm in an argon atmosphere. 1mm ball milling for 2 hours to obtain raw silicon particles.
[0124] Heat treatment: Put the above-mentioned raw material silicon particles into a tube furnace, flow argon-hydrogen mixed gas (hydrogen volume content is 2%), flow rate is 100 sccm, heat treatment at 1000° C. for 2 hours.
[0125] Pickling: immerse the heat-treated raw silicon particles in acid solution, add 0.3 kg of raw silicon particles per liter of acid solution, heat and magnetically stir, and react at 60°C for 5 hours. Then put the acid solution containing the raw silico...
Embodiment 2
[0142] In order to study the influence of the average particle size of raw silicon particles on the purification effect, embodiment 2 obtained raw silicon particles (0.5 micron to 500 micron) with different average particle sizes by controlling the ball milling process (such as ball milling time, ball milling speed and ball diameter). ). These raw silicon particles were subjected to the same heat treatment steps and pickling steps as in Example 1 to obtain purified silicon particles, which were numbered PS-2 to PS-6. At the same time, the purified silicon particles in Example 1 are numbered PS-1.
[0143] The silicon content and impurity content (impurities include Fe, Al, Ca, Mn, Mg, Ti, Cu, B and P) in the PS-1 to PS-6 purified silicon particles were detected by ICP-MS, as shown in Table 4 . The table records the average particle size of the raw silicon particles, the particle size value distribution range of the particle size frequency distribution curve, the total impuri...
Embodiment 3
[0149] The raw silicon granules were obtained according to the method of Example 1, without the step of heat treatment, the raw silicon granules were directly immersed in the acid solution, and the same pickling step as in Example 1 was carried out. Other parameters and steps refer to Example 1 to obtain the purified silicon particles of Example 3.
[0150] ICP-MS detection data shows that the weight content of impurities (including Fe, Al, Ca, Mn, Mg, Ti, Cu, B and P) in the purified silicon particles is 0.008%. The weight content of silicon element in the purified silicon particles is 99.992%.
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