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Direct oxidation refining purification method for industrial silicon melt

An oxidative refining and industrial silicon technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problem of poor removal of element P, and achieve the effects of low cost, high removal rate and low investment

Inactive Publication Date: 2009-07-15
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

AlemanyC, a joint laboratory of France and Canada, published a paper "Refining of metallurgical-grade silicon by inductive plasma" (2002, 72(1-4): 41-48) on "Sol.Energy Mater.Sol.Cells", etc. using plasma flame Gas blowing refining, this method has a good removal efficiency for many impurities in silicon, especially the removal of Al, Ca, Fe, B and other elements is very obvious, but the removal effect of element P is poor, this is because P Easily form non-volatile Si with Si 2 P, SiP phase, when there is more Ca in the melt, it will also combine into a stable compound Ca 4 (PO 4 ) 2 (OH)

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0015] Example 1: 5 kg of molten industrial silicon with a purity of more than 98 wt% was added to the graphite crucible of the heating blowing furnace through a tundish, and the temperature of the silicon melt was kept at 1450-1500° C. by medium frequency induction heating. First, blowing compressed air and 55 wt% SiO into the silicon melt 2 -A gas-solid mixture composed of 45% by weight of CaO, the gas-solid volume ratio is 40:1, the flow rate of the gas-solid mixture is 10L / min, silicon metal elements such as Al, Ca, Ti, Na, Mg are removed, and the refining time is 1h, Remove the slag phase from the surface of the molten silicon; then turn off the compressed air, blow a mixed gas of Ar and 10% by volume of water vapor into the melt, the gas flow rate is 10L / min, the temperature is controlled at 1550°C, the system pressure is 90000Pa, and the blowing time is For 1.5h; change to blowing into Ar+(10vol%)H 2 The mixed gas, the gas flow rate is 10L / min, the melt temperature is ...

Embodiment 2

[0016] Example 2: 5 kg of molten industrial silicon was added to the graphite crucible of the heating blowing furnace through a tundish, and the temperature of the silicon melt was kept at 1450-1500° C. by medium-frequency induction heating. First, blowing compressed air and 60% SiO into the silicon melt 2 -A gas-solid mixture composed of 40% CaO, the gas-solid volume ratio is 30:1, the flow rate of the gas-solid mixture is 15L / min, and silicon metal elements such as Al, Ca, Ti, Na, Mg, etc. are removed, and the refining time is 1h. The slag phase is removed from the molten silicon surface; then the compressed air is turned off and Ar-(15% by volume)H is blown into the melt 2 Mixed gas of O, gas flow rate 10L / min, temperature controlled at 1550°C, system pressure 90000Pa, blowing time 1.5h; change to blowing Ar+(20% volume) H 2The mixed gas, the gas flow rate is 10L / min, the melt temperature is still controlled at 1550°C, the system pressure is 90000Pa, and the blowing time i...

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PUM

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Abstract

The invention relates to a directly oxidizing refining and purifying method for industrial silicon melt, which comprises the following steps: adding melt state industrial silicon into a graphite crucible of a heating converting furnace through a pouring box, keeping the temperature of the silicon melt between 1450 and 1600 DEG C by adopting the intermediate sensing heating way, blowing the gas-solid mixture of compressed air and SiO2-CaO slag oxidant powder into the silicon melt to be oxidized and refined, removing most part of metallic impurity Al, Ca, Ti and the like and a small amount of impurity element B; and then closing the compressed air, blowing oxidized gas H2O steam, removing the residual metallic impurity and non-metallic impurity B; and finally, blowing H2 to remove the impurity element P in silicon. The invention achieves the purposes of reducing metallic impurity in the silicon to be less than 1.0 ppmw, reducing the non-metallic impurities B and P respectively to be less than 0.2 ppmw and 0.5 ppmw, and increasing the t electric resistivity to be larger than 2.5 Omega*cm.

Description

1. Technical field [0001] The invention relates to a method for directly oxidizing, refining and purifying industrial silicon melt, and belongs to the technical field of purifying industrial silicon materials by metallurgical methods. 2. Background technology [0002] Industrial silicon (MG-Si) mainly contains metal impurities such as Fe, Al, Ca and non-metallic impurities such as B, P, C, O, etc. The purity is generally above 98%, and the total content of impurities is usually higher than 10000ppm; solar-grade silicon The purity requirement of (SoG-Si) is 5N~7N. In order to ensure the required photoelectric conversion efficiency, the total impurity content in silicon should not exceed 50ppmw, usually Fe, Al, Ca and other metal impurities are below 5.0ppmw, B, P impurities are low At 1.0ppmw, C, O, etc. are below 5.0ppmw. In order for solar-grade silicon to be widely used, low-cost and high-volume production processes must be used. [0003] In 2007, global solar photovolta...

Claims

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Application Information

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IPC IPC(8): C01B33/037
Inventor 戴永年马文会杨斌伍继君王飞刘大春徐宝强谢克强周阳姚耀春郁青春秦博曲涛邓勇熊恒汪竞福刘永成周晓奎
Owner KUNMING UNIV OF SCI & TECH
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