Method for preparing high-purity silicon by high temperature gas-solid reaction
A solid reaction, high-purity technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of high energy consumption and long process, and achieve simple impurity removal process, low environmental pressure, and low power consumption Effect
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[0032] Example 1
[0033] Using industrial silicon with a purity of 95%-99.99% as raw material, the main impurity component Fe content is 2731ppmw, Al content is 1472ppmw, Ca content is 191ppmw, and Cu content is 59ppmw.
[0034] Preliminarily crush and sieve the raw materials, take a sample with a particle size of 5±1mm, put it on the hearth of the high-temperature solid-phase reaction furnace with a mesh structure, and evacuate it to 1.0×10 -2 Pa to remove the air in the furnace, after inert gas replacement, the inert gas is any one or a mixture of helium, neon, argon, etc., the sample is heated to 1380 ° C, filled with hydrogen, chlorine, fluorine gas , hydrogen chloride, hydrogen fluoride, bromine or hydrogen bromide as active gas, adjust the vacuum to 0.8 × 10 3 Pa is subjected to gas-solid reaction treatment, and the treatment time is 1h, 2h, 4h, 8h and 12h respectively, and any one of hydrochloric acid, hydrofluoric acid, nitric acid or perchloric acid is used to clean...
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[0036] Example 2
[0037] Using industrial silicon with a purity of 95%-99.99% as raw material, the main impurity component Fe content is 2731ppmw, Al content is 1472ppmw, Ca content is 191ppmw, and Cu content is 59ppmw.
[0038] Preliminarily crush and sieve the raw materials, take a sample with a particle size of 10±1mm, put it into a high-temperature solid-phase reaction furnace with a hole-shaped hearth, and evacuate it to 1.0×10 -3 Pa to remove the air in the furnace, after inert gas replacement, the inert gas is any one or a mixture of helium, neon, argon, etc., the sample is heated to 1380 ° C, filled with hydrogen, chlorine, fluorine gas , hydrogen chloride, hydrogen fluoride, bromine or hydrogen bromide as active gas, adjust the vacuum to 0.8×10 4 Pa is subjected to gas-solid reaction treatment, and the treatment time is 1h, 2h, 4h, 8h and 12h, respectively. After washing, washing with water and drying, high-purity silicon with a purity higher than 99.999% is obtain...
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[0040] Example 3
[0041]Using industrial silicon with a purity of 95%-99.99% as raw material, the main impurity component Fe content is 2731ppmw, Al content is 1472ppmw, Ca content is 191ppmw, and Cu content is 59ppmw.
[0042] Preliminarily crush and sieve the raw materials, take a sample with a particle size of 30±1mm, put it into a high-temperature solid-phase reaction furnace with a mesh-like structure, and evacuate it to 1.0×10 -4 Pa to remove the air in the furnace, after inert gas replacement, the inert gas is any one or a mixture of helium, neon, argon, etc., the sample is heated to 1380 ° C, filled with hydrogen, chlorine, fluorine gas , hydrogen chloride, hydrogen fluoride, bromine or hydrogen bromide as active gas, adjust the vacuum to 1.3 × 10 5 Pa, carry out gas-solid reaction treatment, the treatment time is 1h, 2h, 4h, 8h, 12h and 24h and 36h (not shown in the figure), the silicon material after the gas-solid reaction is treated with hydrochloric acid, hydrofl...
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