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Method for refining and purifying electronic-grade silane in polysilicon production process

A technology of production process and purification method, which is applied in the direction of silicon hydride, etc., can solve the problems that the purity is difficult to reach a high standard, silicon tetrachloride cannot be recycled, and energy consumption is high.

Active Publication Date: 2010-09-01
ZHEJIANG ZHONGNING SILICON IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the process is mature, but it also has its disadvantages, such as high energy consumption, the power consumption is 350-500 degrees / kg; the reduction conversion rate is low, only about 15%; The purity is 99.999%-99.9999% (technically called five 9 to six 9); at the same time, the pollution is relatively large, and the tail gas contains a large amount of silicon tetrachloride, which cannot be recycled, and accumulates more and more, forming an environmental protection problem that is difficult to solve

Method used

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  • Method for refining and purifying electronic-grade silane in polysilicon production process
  • Method for refining and purifying electronic-grade silane in polysilicon production process
  • Method for refining and purifying electronic-grade silane in polysilicon production process

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Put the crude silane into the light removal tower through the silane compressor, and remove nitrogen, methane, and hydrogen under the conditions that the temperature at the top of the light removal tower is -120 ° C, the pressure is 1.85 MPa, and the operating pressure difference is 0.5 kPa; The liquid silane is passed into the first weight-removing tower, and ethane, ethylsilane, diethylsilane, boron, Phosphorus; the silane gas discharged from the top of the tower passes through a three-stage adsorption tower, which is equipped with 4A molecular sieves, and the operating pressure of the adsorption tower is 1.6MP to remove ethylene; the purified silane gas comes out of the adsorption tower and enters the second weight removal tower , under the condition that the temperature at the top of the tower is -70°C, the pressure is 1.6MPa, and the operating pressure difference is 1kPa, ethyl silane is removed, and the pure silane gas leaves the top of the second weight removal to...

Embodiment 2

[0030] Put the crude silane into the light removal tower through the silane compressor, and remove nitrogen, methane, and hydrogen under the conditions of the top temperature of the light removal tower being -80°C, the pressure of 2.5 MPa, and the operating pressure difference of 5 kPa; the liquid at the bottom of the light removal tower Silane is passed into the first weight removal tower, and the temperature at the top of the tower is -40°C, the pressure is 2.49MPa, and the operating pressure difference is 15kPa to remove ethane, ethylsilane, diethylsilane, boron, and phosphorus at the bottom of the tower. The silane gas discharged from the top of the tower is passed through a three-stage adsorption tower, the adsorption tower is equipped with 4A molecular sieve, and the operating pressure of the adsorption tower is 2.3MP to remove ethylene; the purified silane gas enters the second weight removal tower from the adsorption tower, Ethyl silane is removed under the condition th...

Embodiment 3

[0034] Put the crude silane into the light removal tower through the silane compressor, and remove nitrogen, methane, and hydrogen under the conditions that the temperature at the top of the light removal tower is -120 ° C, the pressure is 2.2 MPa, and the operating pressure difference is 2.0 kPa; The liquid silane is passed into the first weight-removing tower, and ethane, ethylsilane, diethylsilane, boron, Phosphorus; the silane gas discharged from the top of the tower passes through a three-stage adsorption tower, which is equipped with 4A molecular sieves, and the operating pressure of the adsorption tower is 1.8MP to remove ethylene; the purified silane gas comes out of the adsorption tower and enters the second weight removal tower , under the condition that the temperature at the top of the tower is -60°C, the pressure is 1.6MPa, and the operating pressure difference is 8kPa, ethyl silane is removed, and the pure silane gas leaves the top of the second weight removal tow...

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Abstract

The invention discloses a method for refining and purifying electronic-grade silane in a polysilicon production process, which comprises the following steps of: 1) introducing crude silane into a lightness-removing column of which an operating pressure is 1.8 to 2.5 MPa and a top temperature is -120 to -80 DEG C, and removing nitrogen, methane and hydrogen from the top of the column; 2) making the crude silane flow out from the bottom of the column and enter a first weight-removing column of which the operating pressure is 1.8 to 2.5 MPa and the top temperature is -70 to -40 DEG C, and removing ethane, boron, phosphorus and the like from the bottom of the column; 3) making the silane exhausted from the top of the column enter series-wound absorption columns of which the operating pressures are all 1.6 to 2.3 MPa, and removing ethylene; and 4) making the silane enter a second weight-removing column of which the operating pressure is 1.6 to 2.3 MPa and the top temperature is -70 to 40 DEG C, and removing ethyl silicane. In the silane refined and purified by the method, the content of the nitrogen, the methane and the hydrogen is reduced to be below 1.5*10-9 and the content of the ethane, the ethyl silicane, diethylsilane, the boron and the phosphorus is reduced to be below 2.5*10-9; and the purity of the crude silane can be finally increased to be over 99.9999999 percent, which meets using requirements of electronics industry and semiconductor industry.

Description

technical field [0001] The invention relates to a compound preparation method, in particular to a method for refining and purifying electronic-grade silane in the production process of polysilicon. Background technique [0002] Polycrystalline silicon material is the most basic and main functional material in the electronic information industry and solar photovoltaic power generation industry. With the development of electronic information industry and solar photovoltaic new energy industry, the demand for polycrystalline silicon products will continue to increase. [0003] At present, the polysilicon production process of most enterprises in my country is the improved Siemens method, which actually uses trichlorosilane as the raw material to reduce polysilicon. The advantage of this method is that the process is mature, but it also has its disadvantages, such as high energy consumption, the power consumption is 350-500 degrees / kg; the reduction conversion rate is low, only ...

Claims

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Application Information

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IPC IPC(8): C01B33/04
Inventor 杨建松陈德伟栗广奉耿金春吴希湖
Owner ZHEJIANG ZHONGNING SILICON IND
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