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Method for preparing solar-grade silicon

A solar-grade, silicon powder technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of high energy consumption, high equipment performance requirements, increase production costs, etc., and achieve easy large-scale production and construction cycle. Short, low production cost effect

Inactive Publication Date: 2009-02-04
陕西威斯特硅业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Process technical parameters, especially its important technical parameters are still uncertain, at least its technology has not been fully disclosed;
[0005] 2. The scale of the embodiment is small, indicating that its technology has not yet reached the level of industrialized production;
[0006] 3. The process is complicated, and plasma and electron beams are used in the process, which consumes a lot of energy and requires high equipment performance;
[0007] 4. In order to achieve the target quality, repeated purification operations are required, which increases the production cost
[0008] The inventor of the present invention has disclosed a production method of ultra-pure metallurgical silicon with the total amount of impurities less than 100ppma in the invention patent "A Preparation Method of Ultra-Pure Metallurgical Silicon" application number 200810068852.9, but it still cannot achieve solar energy The requirements for silicon with high-grade purity, that is, B0.3Ω.cm, and total impurities below 10ppma, the inventor applied No. 200810068852.9 on the basis of further research, improving the process conditions of the original method, using a special slagging agent, using physical metallurgical technology, to produce silicon with a quality that meets the requirements of solar-grade purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: (following example does not limit the present invention)

[0019] A preparation method of solar grade silicon, the steps are:

[0020] (1) Grinding and ball milling 200Kg of 99.5% metallurgical silicon to a particle size of 100 mesh; (2) Soaking the silicon powder in 300Kg of 10% hydrochloric acid solution for 24 hours, centrifugal filtration and separation, and washing with pure water until the pH is neutral; (3) dry the silicon powder after wet purification in a vacuum drying oven; (4) mix 150Kg of dried silicon powder with 150Kg of compound slagging agent and put it into a 250L graphite crucible , the graphite crucible is placed in a furnace with a jacketed graphite heating element; wherein the compound slagging agent is made of Na 2 O-CaO-SiO 2 Department and NH 4 Composition of F series, the mass ratio of the two slagging systems is 12:1, Na 2 O-CaO-SiO 2 Department of molar ratio 0.5:1:1, NH 4 F: NH 4 Cl: (NH 4 ) 2 SO 4 The mass ratio of th...

Embodiment 2

[0022] A preparation method of solar grade silicon, the steps are:

[0023] (1) Pulverize 200Kg of 99.5% silicon block and ball mill it to a particle size of 100 mesh; (2) Soak the silicon powder in 300Kg of 12% hydrochloric acid solution for 24 hours, separate by centrifugal filtration, and wash with pure water to neutral pH; (3) dry the silicon powder after wet purification in a vacuum oven; (4) mix 80Kg of dried silicon powder with 160Kg compound slagging agent and put it into a 200L quartz crucible, The quartz crucible is placed in a furnace with a jacketed graphite heating element; the compound slagging agent described therein is made of Na 2 O-CaO-SiO 2 Department and NH 4 Composition of F series, the mass ratio of the two slagging systems is 10:1, Na 2 O-CaO-SiO 2 Department of molar ratio 1:1:1, NH 4 F: NH 4 cl:(NH 4 ) 2 SO 4 The mass ratio is 1:1:0; (5) Start the power supply for induction heating, and at the same time blow protective gas argon into the furna...

Embodiment 3

[0025] A preparation method of solar grade silicon, the steps are:

[0026](1) 100Kg 99.5% metallurgical silicon is pulverized and ball milled to a particle size of 200 mesh; (2) The silicon powder is put into 150Kg of 10% hydrochloric acid solution and soaked for 24 hours, separated by centrifugal filtration, and washed with pure water to neutral pH; (3) dry the silicon powder after wet purification in a vacuum oven; (4) mix 50Kg of dried silicon powder with 30Kg compound slagging agent and put it into an 80L quartz crucible, The quartz crucible is placed in a furnace with a jacketed graphite heating element; the compound slagging agent described therein is made of Na 2 O-CaO-SiO 2 Department and NH 4 CL composition, the mass ratio of the two slagging systems is 12:1, Na 2 O: CaO: SiO 2 Molar ratio 0:1:1, NH 4 F: NH 4 cl:(NH 4 ) 2 SO 4 The mass ratio is 1:3:0; (5) Start the power supply for induction heating, and at the same time blow protective gas nitrogen into the...

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PUM

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Abstract

The invention relates to a preparation method of silicon with solar-grade purity, and provides a preparation method of the silicon with total impurity content less than 10ppma, B less than 2ppma, P less than 6ppma and resistivity more than 0.3omega.cm. The method comprises the following steps: taking industrial silicon powder as the raw material; uniformly mixing the silicon powder and remixed fluxing mediums to be filled into a silica pot inside an induction melting furnace after simple chemical pretreatment; blowing protection gas into the melting furnace under micro vacuum or normal pressure; heating by induction until the temperature inside the furnace reaches 1450 DEG C to 1700 DEG C; melting the metal silicon into silicon melt; removing formed slag. The method can effectively reduce the content of B in the silicon, thus leading B to be less than 2ppma and meeting the ordinary demands of silicon materials of the novel process in manufacturing low-cost solar battery. Moreover, the method has the advantages of simple production process, low production cost, easy large-scale production, small investment and short construction period.

Description

Technical field: [0001] The invention relates to a method for preparing solar-grade silicon, which belongs to the technical field of silicon purification. More specifically, the invention relates to a method for removing impurities from molten silicon by slag-forming treatment in an induction melting furnace. Background technique: [0002] The requirement for silicon to be used in solar cells has a purity of 9 to 6 out of 5. The allowable content varies with the elements. Recently, a breakthrough has been made in a new technology for preparing solar cells using metallurgical silicon. The allowable amount of impurity elements in raw silicon is lower than that required for traditional crystalline silicon solar cells. Generally, the total content of impurities in raw silicon is required to be less than 10ppma. B<2ppma, P<6ppma, resistivity>0.3Ω.cm, and the solar cell conversion efficiency can reach 14%, and the solar cell produced by the new process is lower in cost t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/037
Inventor 吴展平
Owner 陕西威斯特硅业有限公司