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Method for preparing nanometer silicon based on introduction of metal into metallothermic reduction

A metal heat, nano-silicon dioxide technology, applied in non-metallic elements, chemical instruments and methods, silicon compounds, etc., can solve the problems of poor uniformity and dispersion of nanostructures, affecting performance, etc., and achieve uniform appearance and morphology. Improved performance, uniform pore size distribution

Active Publication Date: 2017-03-15
湖南宸宇富基新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, for magnesium thermal or aluminothermic reduction, although porous silicon with nanostructure can be obtained after reduction, the nanostructure of its nanostructure is due to the disordered accumulation of silicon atoms in the reduction process and the fusion of nanostructures. Poor homogenization and dispersion, which affects their performance in specific applications

Method used

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  • Method for preparing nanometer silicon based on introduction of metal into metallothermic reduction
  • Method for preparing nanometer silicon based on introduction of metal into metallothermic reduction
  • Method for preparing nanometer silicon based on introduction of metal into metallothermic reduction

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Effect test

Embodiment 1

[0058] (1) Ethanol is used as a dispersant, and ethyl orthosilicate and zinc nitrate are mixed according to the ratio of zinc:silicon molar ratio of 1:4 to obtain a mixed solution 1, and ammonia water and water having a volume three times that of the mixed solution 1 are mixed. Add the mixed solution with ethanol (the volume ratio of 25% ammonia water, ethanol and water is 9:16:25) slowly into this mixed solution 1, stir at 500r / min at room temperature for 5h, filter and wash with water until neutral, and place in an oven at 80°C After drying, a silicon dioxide / zinc oxide composite precursor is obtained.

[0059] (2) Take 1g of silicon dioxide / zinc oxide composite precursor, mix it with 10g of sodium chloride, add 0.9g of metal magnesium powder, put it in a sealed tube furnace, and raise the temperature at 5°C / min to Insulate at 700°C for 10h, cool the product and treat it in 1mol / L hydrochloric acid for 6h, filter the filter residue and then treat it in 5wt% hydrofluoric acid...

Embodiment 2

[0062] (1) Methanol is used as a dispersant, and methyl orthosilicate and zinc nitrate are mixed according to the ratio of zinc:silicon molar ratio of 1:4 to obtain a mixed solution 1, and ammonia water and water having a volume three times that of the mixed solution 1 are mixed. Add the mixed solution with methanol (the volume ratio of 25% ammonia, ethanol and water is 9:16:25) slowly into this mixed solution 1, stir at room temperature at 500r / min for 5h, filter and wash with water until neutral, and place in an oven at 80°C After drying, a silicon dioxide / zinc oxide composite precursor is obtained.

[0063] (2) Take the above 1g silicon dioxide / zinc oxide composite precursor, mix it with 5g sodium chloride and 5g potassium chloride, then add 0.8g metal magnesium powder, place it in a sealed tube furnace, and heat it under an argon atmosphere 2°C / min to 650°C for 10h, after cooling, the product was treated in 2mol / L hydrochloric acid for 6h, and the filtered residue was trea...

Embodiment 3

[0066] (1) Ethanol is used as a dispersant, and ethyl orthosilicate and zinc nitrate are mixed according to the ratio of zinc:silicon molar ratio of 1:8 to obtain mixed solution 1. Add the mixed solution with ethanol (the volume ratio of 28% ammonia water, ethanol and water is 9:16:25) slowly into this mixed solution 1, stir at 500r / min at room temperature for 5h, filter and wash with water until neutral, and place in an oven at 80°C After drying, a silicon dioxide / zinc oxide composite precursor is obtained.

[0067] (2) Take the above 1g silicon dioxide / zinc oxide composite precursor, mix it with 5g sodium chloride and 5g potassium chloride, then add 0.8g metal magnesium powder, place it in a sealed tube furnace, and heat it under an argon atmosphere 2°C / min to 650°C for 10h, after cooling, the product was treated in 2mol / L hydrochloric acid for 6h, and the filtered residue was treated in 10wt% hydrofluoric acid for 0.5h, filtered and washed until neutral, and dried at 80°C ...

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Abstract

The invention discloses a method for preparing nanometer silicon based on introduction of metal into metallothermic reduction. The method comprises the steps of utilizing a metal ion solution and a liquid silicon source as raw materials, obtaining nano silica-metal oxide precursor through co-deposition, then mixing the precursor and a metallothermic reduction reducing agent, controlling reaction conditions, and removing introduced metal after the metallothermic reduction so as to prepare nanometer silicon particles with various shapes and appearances. Because of the porous structure of the precursor, infiltration of reducing agent metal in the reduction process is promoted, and thus the reaction can be conducted more evenly. The microstructure of the reaction product can be adjusted by adjusting types and quantities of metal. Therefore, the nanometer silicon particles has the advantages of being uniform in appearance and shape, homogeneous in aperture distribution, high in specific surface area and low in preparing cost. According to the method, silicon sources of water glass and the like are metal slat are adopted as raw materials, the method is low in cost, amplifying production is easily achieved, and the method has a wide application prospect in the fields of lithium ion battery materials and the like.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic nano-materials, and in particular relates to a method for preparing nano-silicon based on metal-intervened metal thermal reduction. Background technique [0002] Silicon with nanostructures has broad application prospects in new energy materials, solar energy, microelectronics, biochemistry, and environmental protection. Traditional carbothermal reduction can obtain metallurgical silicon with high purity. However, because the reaction temperature is often above 1400 degrees, it is difficult to obtain widely applicable nano-scale silicon materials. At present, the methods for preparing nano-silicon materials mainly include chemical or electrochemical etching, rapid cooling, laser ablation, reduction of silicon tetrachloride and silane pyrolysis. These preparation methods generally have the disadvantages of high cost, complex equipment, high toxicity and low yield, which are not conducive to...

Claims

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Application Information

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IPC IPC(8): C01B33/023H01M4/38
CPCC01B33/023C01P2002/74C01P2004/04C01P2006/12C01P2006/17H01M4/386Y02E60/10
Inventor 杨娟周向阳任永鹏聂阳陈松吴李力
Owner 湖南宸宇富基新能源科技有限公司
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