Method for preparing crystalline silicon by direct electrolysis in ionic liquid at low temperature

An ionic liquid, crystalline silicon technology, applied in the field of electrolysis, can solve problems such as limited application and high volatility

Inactive Publication Date: 2015-07-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in order to overcome the low boiling point and high volatility of the PC system, the experiment was carried out at a high pressure of 2.6Mpa, which limited the industrial application of this method

Method used

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  • Method for preparing crystalline silicon by direct electrolysis in ionic liquid at low temperature
  • Method for preparing crystalline silicon by direct electrolysis in ionic liquid at low temperature
  • Method for preparing crystalline silicon by direct electrolysis in ionic liquid at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] SiCl 4 dissolved in [N 4441 TFSI] in the ionic liquid, the active material concentration is 0.1M, the working electrode is 100% liquid gallium, the auxiliary electrode is a glassy carbon electrode, and the reference electrode is Ag / (10mM AgNO 3 acetonitrile solution). Constant voltage electrodeposition, the working voltage is -1.8V, the temperature is 90°C, after 8 hours of electrodeposition on the liquid electrode to obtain the product silicon, after the product and the liquid electrode are taken out of the electrolyte at the same time, they are washed with DMF for many times to ensure that the ion The liquid is cleaned, and then the crystalline silicon product is enriched into the organic phase with a mixed solution of anhydrous methanol and acetone equal in volume, and the liquid metal electrode is transferred out. A small amount of liquid metal on the surface of the obtained product is removed by boiling in 10% hydrochloric acid solution. Clean the product with wa...

Embodiment 2

[0022] SiBr 4 dissolved in [N 4441 In TFSI] ionic liquid, active material concentration is 0.25M, and working electrode is the gallium of 68%, the indium of 22% and the tin liquid alloy of 10%, auxiliary electrode is platinum electrode, and reference electrode is Ag / (10mM AgNO 3 acetonitrile solution). Constant voltage electrodeposition, the working voltage is -2.0V, the temperature is 100°C, after 10 hours of electrodeposition on the liquid electrode to obtain the product silicon, after the product and the liquid electrode are taken out of the electrolyte at the same time, they are washed with DMF for many times to ensure that the ion The liquid is washed, and then the crystalline silicon product is enriched into the organic phase with a mixed solution of anhydrous methanol and acetone, and the liquid metal electrode is transferred out. A small amount of liquid metal on the surface of the obtained product is removed by boiling in 10% hydrochloric acid solution. Clean the pr...

Embodiment 3

[0024] SiCl 4 Dissolved in [EMIMTFSI] ionic liquid, the active material concentration is 0.05M, the working electrode is 100% liquid gallium, the auxiliary electrode is a glassy carbon electrode, and the reference electrode is Ag / (10mM AgNO 3 acetonitrile solution). Constant voltage electrodeposition, the working voltage is -3.2V, the temperature is 110°C, after 10 hours of electrodeposition on the liquid electrode to obtain the product silicon, after the product and the liquid electrode are taken out of the electrolyte at the same time, they are washed with DMF for many times to ensure that the ion The liquid is cleaned, and then the crystalline silicon product is enriched into the organic phase with a mixed solution of anhydrous methanol and acetone equal in volume, and the liquid metal electrode is transferred out. A small amount of liquid metal on the surface of the obtained product is removed by boiling in 10% hydrochloric acid solution. Clean the product with water and ...

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Abstract

The invention discloses a method for preparing crystalline silicon by direct electrolysis in an ionic liquid at low temperature, used for solving the existing problem that low temperature cannot be compatible with a crystalline structure in a process of preparing silicon by virtue of an electro-deposition method. The method is characterized in that cubic crystalline silicon can be successfully prepared within a low-temperature range from 90-120 DEG C by taking a low-temperature ionic liquid as an electrolytic solution and liquid metal and alloy thereof as a negative electrode on the basis of the characteristics of the ionic liquid which is low in melting point and not easy to volatilize as well as the dissolution-precipitation balance of silicon in a liquid metal electrode. The method disclosed by the invention has the following characteristics: low operation temperature, stable ionic liquid system, and simple and easy processing steps; the method is subjected to constant-current and constant-voltage control and easy for continuous production, and the method can significantly reduce energy consumption and cost in silicon production. The method disclosed by the invention has a good application prospect in the preparation of a semiconductor material.

Description

technical field [0001] The invention belongs to the field of electrolysis and relates to a new method for preparing crystal silicon by low-temperature electrodeposition. Background technique [0002] Silicon is abundant in nature, and because of its excellent chemical stability, optical properties and semiconductor properties, it is widely used in various fields of optoelectronic technology. At present, in the production process of elemental crystal silicon in industry, the steps are to first mix quartz stone or silica (SiO 2 ) to obtain coarse silicon powder by carbothermal reduction, which has serious pollution and high energy consumption. According to different uses, the obtained silicon powder is further purified by Dupont method, Bell method or Siemens method to obtain single crystal silicon or polycrystalline silicon, which includes the preparation, purification, reduction or decomposition of silicon-containing compounds for industrial silicon These processes also ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B7/12C30B29/06
Inventor 张锁江张军玲陈仕谋董坤张海涛朗海燕高洁
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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