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Polycrystalline silicon centrifugal directional solidification purification method and device

A technology of directional solidification and polysilicon, which is applied in the growth of polycrystalline materials, chemical instruments and methods, and single crystal growth, etc. It can solve the problems of energy consumption costs, difficulty in taking into account the purification efficiency, impurity that cannot be diffused quickly and uniformly, and restricts large-scale production applications, etc. problems, to achieve the effect of reducing the effective segregation coefficient of impurities, stabilizing the purification effect and enhancing the operation safety

Pending Publication Date: 2021-11-02
宁夏红日东升新能源材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these existing methods more or less have the problems of high energy consumption and low efficiency. The DSS Bridgman method uses quantitative addition of raw materials in the same crucible for smelting, and then realizes directional solidification molding by controlling the temperature gradient to dissipate heat. , the crystal growth rate is slow at 0.8-1.0mm / min, the solid-liquid interface remains macroscopically static, the impurities discharged from the solid cannot be quickly and evenly diffused into the liquid, and the effect of removing impurities at one time is not good; EMCP electromagnetic continuous casting method combines cold crucible induction melting and Continuous casting technology can effectively improve the purification effect and shorten the production cycle, but the use of water-cooled copper crucible will inevitably consume a large amount of induction heat energy, which is not conducive to the reduction of energy consumption; although the FZ zone melting and refining method and the CZ crystal pulling method are not professionally used Polysilicon is purified, but it has the function of directional solidification. It has no forced refrigerant, and the solidified crystal is long cylindrical, with long growth cycle and high energy consumption (about 30Kwh / Kg). The ratio (V / S) is also small, which is not conducive to the effective discharge of impurities
Based on this, the conventional directional solidification method for polysilicon purification technology and equipment is difficult to balance energy consumption and purification efficiency, which restricts its large-scale production and application in the field of metallurgical solar-grade polysilicon production technology

Method used

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  • Polycrystalline silicon centrifugal directional solidification purification method and device
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  • Polycrystalline silicon centrifugal directional solidification purification method and device

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Using purity 2N grade industrial silicon as raw material, it is purified by centrifugal directional solidification.

[0044] (1) Put 200 kg of solid silicon material in the crucible body 6, raise the crucible to the main furnace chamber 11, open the vacuum system for gas replacement and vacuuming, fill in protective argon, maintain the furnace pressure at 10000-12000Pa, and open The power switch of the graphite heater 9, the furnace temperature rises to 1550°C and is maintained, and after the solid silicon material is completely melted, the heating power is reduced, and the furnace temperature is controlled to 1450-1480°C.

[0045] (2) Turn on the power supply of the wedge-shaped pulley rotating mechanism 20 of the cooling body 2, set the rotation speed to 30r / min, and pass a large flow of circulating refrigerant argon into the cooling body from the interface of the magnetic fluid sealing body 19, and turn on the main and auxiliary The two vacuum gate valves 23 between ...

Embodiment 2

[0052] Using purity 4N grade industrial silicon as raw material, it is purified by centrifugal directional solidification.

[0053] The process operation steps are the same as in Example 1, only the process parameter of the rotation speed of the cooling body 2 is changed, which is set to 60r / min.

[0054] Purified silicon materials S2a, S3a...S15a and S1b, S2b, S3b...S15b are obtained.

[0055] The purified silicon material obtained in this embodiment all reaches 7N grade purity through testing and testing, that is, the sum of Fe, Al, Ca, Cr, Ni, Cu, Zn metal impurities is less than 0.1 ppm.

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Abstract

The invention discloses a polycrystalline silicon centrifugal directional solidification purification method and device. A rotary centrifugal directional solidification principle is adopted, that is, a cooling body with a circulating refrigerant introduced into a middle cavity is inserted into molten silicon liquid at a certain rotating speed, and due to the fact that a large temperature gradient exists between the cooling body and the molten silicon liquid, the silicon liquid can solidify a layer of crystals with high purity on the cooling body, and after a period of time, the cooling body and the crystals rise together and are separated by virtue of external force, so that the purpose of rapid and efficient purification is achieved. According to the method for preparing the polycrystalline silicon with the purity of 6-7 N grade by taking the 2-4 N grade industrial silicon as the raw material, the invention provides the directional solidification purification device and the directional solidification method for the metallurgical solar grade polycrystalline silicon, and the device has the characteristics of large single-furnace productivity, good impurity removal effect, continuous production, short process time and low operation energy consumption, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of metallurgical solar-grade polysilicon production, specifically relates to a directional solidification technology for efficiently removing metal impurities in polysilicon, and provides a polysilicon centrifugal directional solidification purification method and device. Background technique [0002] Photovoltaic power generation, green and clean energy, as a way of solar energy utilization, has developed rapidly in recent years. Its main basic material is solar-grade polysilicon (purity ≥ 99.9999%, 6N), which is currently mainly prepared by chemical method-improved Siemens method to purify industrial silicon technology . Metallurgical polysilicon technology is also a method of preparing solar-grade polysilicon. Because of its potential advantages such as low project investment, short process flow, low energy consumption, and environmental friendliness, it has attracted widespread attention from the industr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/06C30B28/06
CPCC30B29/06C30B28/06Y02P20/10
Inventor 徐国林范占军王志钱国余马晓琳孟范兴柳云杨瑞芬曹永柱白宇峰
Owner 宁夏红日东升新能源材料有限公司
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