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Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification 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 reduced industrial production costs, high cost of cutting equipment, and affecting purification effects, etc. The effect of reducing consumption and reducing process links

Inactive Publication Date: 2013-03-20
QINGDAO NEW ENERGY SOLUTIONS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the subsequent slow cooling process, the impurities in the high-concentration area will diffuse to the low-concentration area, 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 tail that needs to be removed The waste is as high as 25%~35%, and the finished product rate is only 65-75%
At the same time, due to the relatively high hardness of silicon, high-power cutting equipment is needed to separate the purified silicon ingot from the ingot tailings with high impurity content at the tail. At present, wire cutting and diamond saw band cutting are generally used for cutting, but cutting The high cost of equipment and the large consumption of saw bands are not conducive to the reduction of industrial production costs. At present, there are few effective methods in China to facilitate the removal of tailings

Method used

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  • Method and equipment for rapid collection and purification of polycrystalline silicon through directional solidification of tailing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] like figure 1 The shown equipment for rapidly collecting and purifying polysilicon from directional solidification tailings is composed of a vacuum chamber 2 to form an outer wall, a vacuum pipeline 15 is installed on the outer wall, and one end of the vacuum pipeline 15 is connected to a vacuum pump group 14. The chamber draws a vacuum.

[0025] A ventilation line 13 is fixedly installed on the outer wall. The ventilation line is used to fill the vacuum chamber with gas, such as inert gas, etc. The water cooling plate 12 is movably installed at the bottom of the vacuum chamber 2. The graphite plate 11 can be raised or lowered according to the set speed. The graphite plate 11 is placed on the top of the water-cooling plate. There are 4 holes on the graphite plate 11. Sleeve connection, the graphite tray is provided with a card slot, which is conducive to the nested connection of the graphite strut with it.

[0026] The crucible 7 is placed on the graphite tray 9, the ...

Embodiment 2

[0033] Using the equipment described in Example 1 to take the tailings and purify polysilicon by directional solidification, firstly add silicon material with a purity of 99.0% cleaned by 90% of the crucible volume into the crucible 7, close the ventilation line 13, open the vacuum pump group 15, and The vacuum degree in the vacuum chamber 2 is pumped to 10Pa, the vacuum pump group 14 is closed, the ventilation pipeline is opened, and 99.91% argon is filled into the vacuum chamber 2, and the pressure reaches 500Pa, and the ventilation pipeline is closed;

[0034] The second step of smelting and solidification: turn on the power supply, use the induction coil 5 and the graphite heating element 6 to heat the silicon material in the crucible 7 to 1450 ° C to completely melt into a silicon melt, and keep it at this temperature for 30 minutes, and pull it vertically downward. The water cooling plate 12 makes the silicon melt in the crucible 7 move vertically downward at a uniform sp...

Embodiment 3

[0037] The equipment described in Example 1 is used to take the tailings and purify polysilicon by directional solidification. First, add silicon material with a purity of 99.3% cleaned by 92% of the crucible volume into the crucible 7, close the ventilation line 13, open the vacuum pump group 15, and The vacuum degree in the vacuum chamber 2 is pumped to 2Pa, the vacuum pump group 14 is closed, the ventilation pipeline is opened, and the purity of 99.96% argon is filled into the vacuum chamber 2, until the pressure reaches 5000Pa, and the ventilation pipeline is closed;

[0038] The second step of smelting and solidification: turn on the power supply, use the induction coil 5 and the graphite heating element 6 to heat the silicon material in the crucible 7 to 1550 ° C to completely melt into a silicon melt, and keep it at this temperature for 45 minutes. Pull down vertically The water-cooling plate 12 makes the silicon melt in the crucible 7 move vertically downward at a unifo...

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Abstract

The invention belongs to the technical field of metallurgy purification, and particularly relates to a method and equipment for directional solidification and purification of polycrystalline silicon through taking tailing. According to the method, under the inert gas shielding environment, abluent silicon is heated to be fully melted so as to carry out directional solidification; ingot pulling is stopped when solidification is completed by 85-90%, a graphite bent pipe is stretched into surplus unset silicon at the upper layer, then the other end of the graphite bent pipe is vacuumed through a vacuum unit, so that the surplus unset silicon at the upper layer enters the graphite bent pipe under the action of pressure difference and enters a water cooling collection box through the guide of the graphite bent pipe; heating is stopped after all the surplus unset silicon at the upper layer enters the water cooling collection box, and cast ingot solidified in a crucible is silicon cast ingot of high purity. Due to the method, back-diffusion of impurity is prevented, technology processes are reduced, and the yield of cast ingot is improved. The equipment is convenient to improve and install, and a tailing collection device can be used repeatedly, can collect more tailings, and is safe and reliable.

Description

technical field [0001] The invention belongs to the technical field of metallurgical purification, and in particular relates to a method and equipment for purifying polycrystalline silicon by tail material extraction type directional solidification. Background technique [0002] The purification of silicon raw materials is an important link in the solar photovoltaic industry chain, and the rapid development of the photovoltaic industry relies on high-efficiency and low-cost purification methods. Directional solidification technology has been widely used in many fields of metal purification, and achieved remarkable results. In the process of purifying silicon raw materials, metal impurities with a segregation coefficient much less than 1 will be enriched in the liquid phase during the directional solidification process and finally removed. This method is one of the key links in the current metallurgical preparation of solar-grade polysilicon, and is the most effective method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/037
Inventor 谭毅姜大川安广野石爽邹瑞洵
Owner QINGDAO NEW ENERGY SOLUTIONS
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