Refining and purifying method for industrial silicon

A technology for refining and purifying industrial silicon, which is applied in the fields of chemical instruments and methods, silicon compounds, inorganic chemistry, etc. It can solve problems such as complex process, no obvious effect of difficult-to-volatile impurity elements, pollution, etc., and achieve high purification effect Effect

Inactive Publication Date: 2015-04-08
QINGHAI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Existing refining and purification processes, such as Elkem process, ARTIST process, Carbothermicmeth process, HEM process, Kawasaki Steel process, improved Siemens method-closed-loop SiHCl 3 Hydrogen reduction method, iodine chemical vapor transmission purification method under normal pressure, zinc reduction method, etc., the process is complicated, the purification effect is unstable, the cost is high, the energy consumption is high, and the pollution is serious
The existing vacuum consumable arc refining can volatilize and remove the gas and some volatile impurity elements in the raw material, but it is difficult to remove the difficult volatile impurity elements Fe, Al, etc.; the existing industrial silicon vacuum distillation refining metal can make the industrial The content of Ca element in silicon is significantly reduced, and it can remove phosphorus from industrial silicon by vacuum distillation, but it has no obvious effect on other difficult-to-volatile impurity elements

Method used

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  • Refining and purifying method for industrial silicon

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Effect test

Embodiment 1

[0023] According to the above-mentioned technical solution of the present invention, the industrial silicon refining and purification method provided in this embodiment includes: figure 1 As shown, in the vacuum electric arc furnace 4, the industrial silicon rod 1 is used as the consumable cathode, and the crucible 2 containing the refining slag 3 is used as the anode. -4 ~10 - 2 Under the vacuum degree of Pa, the industrial silicon rod 1 is gradually melted and dropped onto the refining slag 3 from the lower end, and the C, O, H gas impurities and B, P volatile impurity elements in the industrial silicon molten droplets are volatilized and released, and then The vacuuming device is drawn out of the vacuum electric arc furnace 4 . After the industrial silicon drops onto the refining slag 3, non-volatile Fe, Ca, Ti, Al, V, and Na impurities enter the refining slag 3 through the slag-gold reaction and element exchange. When the industrial silicon rod 1 cathode melting is compl...

Embodiment 2

[0025] The difference between the present embodiment and the first embodiment is that in the present embodiment, the vacuum degree of the vacuum electric arc furnace is 10 -3 ~10 - 2 Pa, temperature is 1600 ~ 1700 ℃. The industrial silicon rods are produced by pressing and sintering industrial silicon crumbs and are refined in a vacuum consumable electric arc furnace with conventional diameters. The initial purity is that the Si content is not less than 99.5%. In the composition of said refining slag, calculated by mass percentage: SiO 2 30-50%, SiC 5-15%, Si 1-10%, MgO 0.1-0.5%, Al 2 o 3 15-25% for CaO, 15-25% for CaO, 0.1-0.5% for FeO, and the purity of silicon after refining reaches 5N.

Embodiment 3

[0027] According to the above-mentioned technical solution of the present invention, the industrial silicon refining and purification method provided in this embodiment includes: figure 1 As shown, in the vacuum electric arc furnace 4, the industrial silicon rod 1 is used as the consumable cathode, and the crucible 2 containing the refining slag 3 is used as the anode. -4 ~10 - 2 Under the condition of Pa vacuum degree, the industrial silicon rod 1 is gradually melted and dropped onto the refining slag 3 from the lower end, and the gas impurities and some volatile impurity elements in the industrial silicon molten drop are volatilized and released, and then the vacuum arc is drawn out by the vacuum device. Furnace 4 outside. After the industrial silicon drops onto the refining slag 3, non-volatile impurities enter the refining slag 3 through the slag-gold reaction and element exchange. After the industrial silicon rod 1 cathode melting is completed, the refining slag is remo...

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Abstract

The invention discloses a refining and purifying method for industrial silicon. The method comprises the following steps: in a vacuum electric arc furnace, using an industrial silicon rod as a consumable negative pole and a conductive crucible as a positive pole, wherein the conductive crucible contains refining slags; after striking the arc for the electric arc furnace under high-temperature and vacuum conditions, the industrial silicon rod is gradually smelted and dropped to a positive pole crucible from the lower end of the consumable negative pole, and gas impurities and volatile impurities in industrial silicon molten drops are volatilized and diffused and are vacuumized out of the furnace by virtue of a vacuumizing device; after the industrial silicon molten drops drop into the positive pole crucible, nonvolatile impurities enter into the refining slags by slag-gold reaction and element exchange; and when the industrial silicon negative pole is molten, the refining slags are removed to obtain the refined and purified industrial silicon. According to the scheme, a high purification effect is achieved. 5-7N purity polycrystalline silicon can be obtained by way of purification.

Description

technical field [0001] The invention relates to the technical field of metallurgical industry, in particular to an industrial silicon refining and purification method. Background technique [0002] In qualified silicon substrates for silicon photovoltaic cells, in addition to C and O impurities, the content of B, P, Fe, Ca, Ti, V, Al, Na and other impurities should be less than 1.0×10 -6 , the concentration of other impurities should be lower than 1.0×10 -9 , Polysilicon of this purity is called solar grade silicon. Purity requirements for solar-grade silicon: First, the total content of impurities should be as low as possible, generally not higher than 100ppm; second, from the perspective of single impurities, Ti, V, B, P, etc. have the greatest impact, and the content must be lower than 1ppm. The purity of industrial silicon is about 95%-99%, and its impurities are mainly non-metallic impurities C, B, P and metal impurities Fe, Al, Ca, etc. If it is used as a solar phot...

Claims

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Application Information

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IPC IPC(8): C01B33/037
Inventor 铁生年陈明彪梅生伟
Owner QINGHAI UNIVERSITY
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