Method for synthesizing high specific surface mesoporous silicon carbide at low temperature and silicon carbide product

A technology of mesoporous silicon carbide and high specific surface, applied in the field of silicon carbide products, low temperature synthesis of high specific surface mesoporous silicon carbide, can solve the problems of low product purity, small specific surface area of ​​silicon carbide materials, pollution, etc., and achieve particle size And the particle distribution is uniform, no secondary pollution, and the effect of simplifying the pickling process

Inactive Publication Date: 2019-11-29
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The common feature of the above synthesis methods is that high temperature reaction is required, and the reaction temperature is generally between 1250 and 1800 °C, which undoubtedly increases the preparation cost and is very unfavorable for the practical application of the material
In addition, the high temperature process will destroy the microscopic morphology and structure of SiC materials, leading to SiC agglomeration, and the prepared silicon carbide materials usually have small specific surface area, low product purity and uneven particle size distribution, which further limit its industrial application.
Therefore, the development of a relatively mild SiC synthesis process has become an urgent problem to be solved. The specific surface area of ​​SiC materials prepared in the prior art is generally lower than 200m 2 / g, a large amount of hydrofluoric acid and other strong corrosive solutions need to be used in the preparation process, and the pollution is serious

Method used

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  • Method for synthesizing high specific surface mesoporous silicon carbide at low temperature and silicon carbide product
  • Method for synthesizing high specific surface mesoporous silicon carbide at low temperature and silicon carbide product
  • Method for synthesizing high specific surface mesoporous silicon carbide at low temperature and silicon carbide product

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Add 5g of deionized water, 3g of ethanol, and 0.5g of HCl solution (1mol / L) into a 100mL polyethylene bottle with a seal and mix well, then add 4.1g of tri-block polymer P123 under stirring conditions for 2 hours until completely dissolved . Then 10 g of TEOS and 5 g of furfuryl alcohol were slowly added into the above mixed solution under vigorous stirring, aged at room temperature for 2 days, and then vacuum-dried at 70° C. for 2 days. The resulting block was taken out and carbonized for 6 hours under the protection of argon to obtain a composite filled with carbon in mesoporous silica. After grinding the above compound, add magnesium powder and mix at a mass ratio of 1:1, and react at 700°C for 6 hours. The resulting product is cleaned in 1mol / L hydrochloric acid solution, and there is no excess SiO in the product 2 There is no need to use strong corrosive liquids such as hydrofluoric acid. Then wash with deionized aqueous solution, after filtering and drying, the...

Embodiment 2

[0041] Add 5g of deionized water, 3g of ethanol, and 0.5g of HCl solution (1mol / L) into a 100mL polyethylene bottle with a seal and mix well, then add 4.1g of tri-block polymer P123 under stirring conditions for 2 hours until completely dissolved . Then 10 g of TEOS and 5 g of furfuryl alcohol were slowly added into the above mixed solution under vigorous stirring, aged at room temperature for 2 days, and then vacuum-dried at 70° C. for 2 days. The resulting block was taken out and carbonized for 6 hours under the protection of argon to obtain a composite filled with carbon in mesoporous silica. After grinding the above compound, add magnesium powder and mix at a mass ratio of 1:2, and react at 700°C for 6 hours. The resulting product is cleaned in 1mol / L hydrochloric acid solution, and there is no excess SiO in the product 2 Therefore, there is no need to use strong corrosive liquids such as hydrofluoric acid, then deionized water solution, liquid cleaning, after filtration...

Embodiment 3

[0043] Add 5g of deionized water, 5g of ethanol, and 1.0g of HCl solution (1mol / L) into a 100mL sealed polyethylene bottle and mix well, then add 3g of triblock polymer P123 under stirring conditions for 2 hours until completely dissolved. Then, 12 g of TEOS and 5 g of furfuryl alcohol were slowly added into the above mixed solution under vigorous stirring, aged at room temperature for 2 days, and then vacuum-dried at 70° C. for 2 days. The resulting block was taken out and carbonized for 6 hours under the protection of argon to obtain a composite filled with carbon in mesoporous silica. After grinding the above compound, add magnesium powder and mix at a mass ratio of 1:3, and react at 650°C for 6 hours. The resulting product is in 2mol / L hydrochloric acid solution, and there is no excess SiO in the product 2 Therefore, there is no need to use strong corrosive liquids such as hydrofluoric acid, and then a deionized aqueous solution is filtered and dried to obtain a mesoporou...

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Abstract

The present invention discloses a method for low-temperature synthesis of a high specific surface mesoporous silicon carbide, and a silicon carbide product thereof. The method comprises: preparing a C / SiO2 precursor by using a triblock copolymer P123 as a templating agent, using tetraethyl orthosilicate as a silicon source and using furfuryl alcohol as a carbon source; and in the presence of an inert gas, carrying out magnesium heat reducing and washing drying on the C / SiO2 precursor to obtain the silicon carbide material, wherein the crystal form is 3C-SiC. According to the present invention, with the method, the preparation temperature is substantially reduced, the reaction temperature can be reduced to less than 700 DEG C, the energy consumption is significantly reduced, and the precursor preparation time is short and only requires about 4 days; the precursor material selects the mutually-supported and interactively-growing C / SiO2 as the precursor, such that the skeleton structure during the reaction process can be retained to the maximal degree, and the specific surface area of the prepared material is large and can achieve 600-800 m<2> / g; and the prepared silicon carbide mesoporous material has characteristics of uniform particle size and uniform particle distribution, and has the size of 10-20 nm.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a method for synthesizing high specific surface mesoporous silicon carbide at low temperature and a silicon carbide product. Background technique [0002] Silicon carbide (SiC), commonly known as emery, has a hardness close to that of diamond, a high band gap, high thermal conductivity, a small dielectric constant and a high electron saturation mobility. Based on its many excellent physical and chemical properties, SiC shows great application prospects in the fields of non-ferrous metal smelting industry, building materials ceramics, energy-saving industry and electronic materials. At present, the main method for preparing SiC in industry is the Acheson method, that is, mixing coke powder and quartz sand and reacting at a high temperature above 2000°C to prepare SiC. Scholars at home and abroad have conducted a lot of research on the preparation of SiC mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/97B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00C01P2002/72C01P2002/82C01P2004/03C01P2004/64C01P2006/12
Inventor 姚建峰张雄飞陈越峰袁林峰
Owner NANJING FORESTRY UNIV
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