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Low-temperature electrolysis of sio using ionic liquids 2 Method for preparing high-purity silicon thin film

A technology of ionic liquid and silicon thin film, which is applied in the field of materials, can solve problems such as poor conductivity, high process energy consumption, and slow reduction rate, and achieve the effects of reducing the thickness of silicon wafers, shortening the process flow, and reducing production energy consumption

Active Publication Date: 2017-03-22
NORTHEASTERN UNIV LIAONING
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AI Technical Summary

Problems solved by technology

[0006] In recent years, many studies have focused on the development of new technologies for the low-cost preparation of solar-grade high-purity silicon, which are divided into the following categories: (1) fluoride systems (such as LiF-KF, NaF-CaF 2 , LiF-KF-NaF, etc.) or chloride system (such as CaCl 2 , NaCl-CaCl 2 -CaO, etc.) as the supporting electrolyte, using silicate or silicon dioxide as the solute to electrodeposit silicon; this process has high energy consumption, discontinuous production, and the use of carbon anodes will bring a certain amount of impurities such as boron and phosphorus into the product silicon, which increases the difficulty for the subsequent physical or chemical purification of silicon; (2) with high-purity SiO 2 As cathode, in CaCl 2 Direct electrodeoxidation in molten salt, solid SiO 2 reduced to silicon; due to SiO 2 The electrical conductivity of the material is poor, resulting in a slow internal reduction rate and incomplete reduction that are not in contact with the cathode conductive filament, and the product Si and the raw material SiO 2 Coexistence, the efficiency is too low; (3) SiCl 4 As a solute, in an ionic liquid (such as 1-ethyl-3-methylimidazole, 1-butyl-2-methylpyrrolidine bisimide, 3-methyl-n-hexylammonium bisimide, etc.) Electrodeposition of Si in medium; due to the silicon source SiCl used 4 is chlorinated or SiO by direct heating of Si 2 Prepared by adding carbochlorination, the reactants of these two chlorination processes Cl 2 and product SiCl 4 Both are toxic substances, requiring additional treatment, long process flow, and high production costs; (4) in organic solvents (such as propylene carbonate, ethylene glycol, a mixture of acetonitrile and tetrahydrofuran, etc.), SiCl 4 / SiHCl 3 Electrodeposition of silicon for solutes
The silicon prepared by this method contains impurities such as C, O, N, and Cl, which cannot meet the purity requirements of solar-grade Si, and there are problems such as weak conductivity of organic solvents, low deposition rate, and volatile electrolytes.

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  • Low-temperature electrolysis of sio using ionic liquids  <sub>2</sub> Method for preparing high-purity silicon thin film
  • Low-temperature electrolysis of sio using ionic liquids  <sub>2</sub> Method for preparing high-purity silicon thin film

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Embodiment 1

[0047] Low-temperature electrolysis of SiO using ionic liquids 2 The structure of the high-purity silicon thin film device is as follows: figure 1 As shown, the electrolytic cell 10 comprising the electric heating jacket 7 and its inside; the electric heating jacket 7 is provided with a thermocouple 5, and the electrolytic cell cover 4 on the top of the electrolytic cell 10 is provided with an inert gas inlet 3 and an inert gas outlet 13; The inside of the tank 10 is provided with a working electrode 6, a counter electrode 11 and a reference electrode 12, and the guide rods of the working electrode 6, the counter electrode 11 and the reference electrode 12 are respectively inserted into the rubber plugs 14 that have been drilled, and then inserted into the electrolytic cell cover. 4, forming a whole, inserted into the inside of the electrolytic cell 10; the top of the electrolytic cell 10 is also provided with a feeder 2, the feeder 2 is filled with silicon dioxide 1, and the ...

Embodiment 2

[0056] Device structure is with embodiment 1, and method is with embodiment 1, and difference is:

[0057] (1) Prepare the raw materials of the electrolyte. The raw materials of the electrolyte are fluorinated imidazolium ionic liquid, cryolite, hydrofluoric acid solution and silicon dioxide, of which fluorinated imidazolium ionic liquid accounts for 96% of the total mass of the electrolyte, and cryolite accounts for the total mass of the electrolyte 1%, silicon dioxide accounts for 1.5% of the total mass of the electrolyte, and hydrofluoric acid solution accounts for 1.5% of the total mass of the electrolyte; the fluorinated imidazole ionic liquid is 1-ethyl-3-methyl fluorinated imidazole;

[0058] (2) Control the electrolyte temperature at 20°C and control the current density at 20mA / cm 2 ; The pole spacing between the working electrode and the counter electrode is 25mm; the effective area S of the working electrode is 200cm 2 ;

[0059] (3) During the electrolysis process...

Embodiment 3

[0063] Device structure is with embodiment 1, and method is with embodiment 1, and difference is:

[0064] (1) Prepare the raw materials of the electrolyte. The raw materials of the electrolyte are fluorinated imidazolium ionic liquid, cryolite, hydrofluoric acid solution and silicon dioxide, of which fluorinated imidazolium ionic liquid accounts for 97% of the total mass of the electrolyte, and cryolite accounts for the total mass of the electrolyte 0.5%, silicon dioxide accounts for 1% of the total mass of the electrolyte, hydrofluoric acid solution accounts for 1.5% of the total mass of the electrolyte; the fluorinated imidazolium ionic liquid is 1-propyl-3-methylimidazolium fluoride;

[0065] (2) Control the electrolyte temperature at 85°C and control the current density at 80mA / cm 2 ; The pole spacing between the working electrode and the counter electrode is 15mm; the effective area S of the working electrode is 200cm 2 ;

[0066] (3) During the electrolysis process, a...

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Abstract

A method for producing high-purity silicon thin films by low-temperature electrolysis of SiO2 using ionic liquids. The following steps are followed: (1) Prepare electrolyte raw materials such as fluorinated imidazole ionic liquid, cryolite, hydrofluoric acid solution and silicon dioxide; (2) The electrolyte is made in the electrolytic cell, and the silicon dioxide is electrolyzed under inert gas circulation and stirring conditions; (3) Add silicon dioxide during the electrolysis process; (4) Replace the working electrode every 1 to 2 hours; (5) Remove the silicon dioxide The film peels off, washed and dried. The method of the invention can electrodeposit silicon at low temperature, and the obtained silicon has high purity; it provides technical reserves for the green preparation of low-cost, low-pollution solar-grade silicon thin films.

Description

technical field [0001] The invention belongs to the field of material technology, in particular to a low-temperature electrolysis of SiO using ionic liquid 2 A method for preparing high-purity silicon thin films. Background technique [0002] The rapid development of industry consumes a large amount of fossil fuels and emits a large amount of greenhouse gases. Under the dual pressure of energy and the environment, the development of renewable energy has become a current hot spot and focus; solar photovoltaic power generation is a renewable energy that countries around the world focus on. One of the technologies with the broadest development prospects. [0003] China is very rich in solar energy resources, with a theoretical reserve of 1.7 trillion tons of standard coal per year; according to my country's current plan, the cumulative installed capacity of photovoltaic power generation in China will reach 600GWp by 2050; The installed capacity of electricity will account for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B1/00
Inventor 徐君莉公维英谢开钰刘爱民李亮星张霞石忠宁
Owner NORTHEASTERN UNIV LIAONING
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