Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing

A technology of directional solidification and polysilicon, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of high cost of cutting equipment, influence on purification effect, unfavorable production cost, etc., achieve convenient equipment transformation and installation, and reduce process links , The effect of saving production cycle and cost

Inactive Publication Date: 2014-08-27
QINGDAO NEW ENERGY SOLUTIONS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, at the end of the solidification of the ingot, impurities are enriched in the melt at the top of the crucible. During the final slow solidification process, the impurities with high content will diffuse to the parts with low impurity content, so that the purity of silicon will gradually decrease with the prolongation of the holding time. , which affects the purification effect, and in this case, the removed tailings are as high as 25%~35%, that is, the yield is only 65-75%, and the hardness of silicon ingots is relatively large, which requires high-power cutting equipment to To separate the purified silicon ingot and the ingot tailings with high tail impurity content, wire cutting and diamond saw band cutting are generally used for cutting at present, but the cost of cutting equipment is high, and the consumption of saw band is large, which is not conducive to the cost of industrial production. reduce, but there are few effective methods in China to facilitate the removal of tailings

Method used

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  • Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] like figure 1 The equipment used in the method for directional solidification and purification of polysilicon by vacuum extraction of tailings is shown. The outer wall is composed of a vacuum chamber 2, and a vacuum pipeline 15 is installed on the outer wall. One end of the vacuum pipeline is connected to a vacuum pump group 14.

[0025] A ventilation pipeline 16 is fixedly installed on the outer wall, and a tailings collection box 13 is installed movably. The water cooling plate 12 is movably installed at the bottom of the vacuum chamber, and the graphite plate 11 is placed on the top of the water cooling plate. One end is nested and connected with the graphite plate through a hole, and the other end is nested and connected with the graphite tray 9. The crucible is placed on the graphite tray, the graphite heating element 6 is set on the periphery of the crucible 7 and fixed on the side wall of the vacuum chamber, and the carbon felt insulation barrel 4 sets are instal...

Embodiment 2

[0032] Use the equipment described in Example 1 to take the tailings and carry out directional solidification to purify polycrystalline silicon. First, add silicon material with a purity of 99.5% to the crucible 7, which is 90% of the volume of the crucible, close the ventilation line 16, and turn on the vacuum pump group 14. The vacuum degree in the vacuum chamber 2 is pumped to 10Pa, then close the vacuum pump group, open the ventilation pipeline 16, fill the vacuum chamber 2 with 99.91% argon until the pressure reaches 100Pa, and close the ventilation pipeline 13;

[0033]The second step of smelting and solidification: turn on the power, use the induction coil and graphite heating element to heat the silicon material in the crucible to 1450°C until it is completely melted into a silicon melt, and keep it at this temperature for 30 minutes, then pull the water cooling plate vertically downward, Make the silicon melt in the crucible move vertically downward at a constant speed...

Embodiment 3

[0036] Use the equipment described in Example 1 to take the tailings and carry out directional solidification to purify polysilicon. First, add silicon material with a purity of 99.6% of the volume of the crucible to the crucible 7, close the ventilation line 16, and turn on the vacuum pump group 14. The vacuum in the vacuum chamber 2 is pumped to 1Pa, then the vacuum pump group is closed, the ventilation pipeline 16 is opened, and 99.95% argon gas is filled into the vacuum chamber 2 until the pressure reaches 1000Pa, and the ventilation pipeline 13 is closed;

[0037] The second step of smelting and solidification: turn on the power, use the induction coil and graphite heating element to heat the silicon material in the crucible to 1550 ° C until it is completely melted into a silicon melt, and keep it at this temperature for 40 minutes, pull the water cooling plate vertically downward, Make the silicon melt in the crucible move vertically downward at a constant speed of 0.9 m...

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Abstract

The method comprises: in an inert gas, melting the silicon material to form silicon melt and insulating; directionally solidifying; stopping ingot pulling when 85-90% of melt is solidified, then diving a quartz tube into the residual silicon melt, vacuum-pumping the other end of the quartz tube by a vacuum-pumping device, pushing the residual silicon melt into the quartz tube under the action of pressure difference, continuously and downwards pulling the ingot, and diving a tailing collecting box below the quartz tube when a crucible departs from a heating zone; cutting off power supply, and stopping heating. After spalling, the quartz tube following the tailing falls down to the collecting box, and the ingot casting obtained in the crucible is high purity silicon ingot casting. The method and the device prevent the diffusion of impurity, reduce technology, and raise yield of the ingot casting. Direct separation of impurity enrichment region is implemented in an end stage of solidification. The device has advantages of convenient reconstruction and installation, and simple operation, can effectively removes the impurity enriched in the tail part of the ingot casting, and saves a production period and cost.

Description

technical field [0001] The invention belongs to the technical field of metallurgical purification, in particular to a method and equipment for extracting tailings and performing directional solidification to purify polysilicon. Background technique [0002] The development of the solar photovoltaic industry relies on the purification of silicon raw materials. In the process of purifying silicon raw materials, the directional solidification method is very important for removing metal impurities with very small segregation coefficients in silicon raw materials. One of the most effective methods, moreover, the directional solidification technique is widely used in metallurgical purification. Directional solidification is the use of forced means to form a temperature gradient in a specific direction in the melt, so that the melt at the low temperature part crystallizes and nucleates, and becomes the starting point for the solidification of the melt. Solidify in the opposite dir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/037
Inventor 姜大川胡志刚安广野谭毅
Owner QINGDAO NEW ENERGY SOLUTIONS
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