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Method for obtaining ordered mesoporous silicon carbide through in-situ conversion of polycarbosilane

A mesoporous silicon carbide and silicon carbide technology, which is applied in the field of material preparation, can solve the problems of the influence of material structure, high specific surface area and low ceramic conversion rate, and achieve the effect of high silicon content and high ceramic conversion rate.

Inactive Publication Date: 2015-09-02
EAST CHINA UNIV OF SCI & TECH
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Problems solved by technology

[0004] However, the currently used polycarbosilane has certain disadvantages. At high temperatures, its ceramic conversion rate is not high and a large amount of free carbon will be produced. The free carbon can form a large number of micropores, resulting in a high specific surface area, which has a negative impact on the structure of the material. certain influence

Method used

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  • Method for obtaining ordered mesoporous silicon carbide through in-situ conversion of polycarbosilane
  • Method for obtaining ordered mesoporous silicon carbide through in-situ conversion of polycarbosilane

Examples

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Embodiment 1

[0026] Example 1, put 1g of pure PCAS into a muffle furnace for curing, and cure at 300°C for 40 hours; put the obtained brown solid in a tube furnace, and bake it in an argon atmosphere at 1400°C for 6 hours to obtain silicon carbide . The Si / C (molar ratio) in the obtained product is 1:1.002.

Embodiment 2

[0027] Example 2, when using powdered SBA-15 as a template, casting PCAS in-situ conversion synthesis of ordered nano-mesoporous silicon carbide materials with a two-dimensional hexagonal structure, the synthesis steps are as follows: put 2.0g of SBA-15 powder into a flask Add 2.0g PCAS and continue vacuuming for 0.5 hours; return to normal pressure and mechanically stir for 1 hour; then put the mixture in an oven and place it at 80°C for 6 hours; when filling for the second time, Polycarbosilane is 1.0 g. Then the obtained dark brown solid was transferred to a muffle furnace and solidified at 250°C for 30 hours; finally, the obtained brown solid was put into a tube furnace and roasted in an argon atmosphere at 1400°C for 6 hours to obtain silicon carbide and Composite of silica. Soak the composite with 4% HF solution for 24 hours, then filter, wash and dry to obtain a black powder, which is the desired ordered nanometer mesoporous silicon carbide material. The nano-mesoporo...

Embodiment 3

[0028] Example 3, when using monolithic SBA-15 with a two-dimensional hexagonal structure as a template, casting PCAS to synthesize ordered nanometer mesoporous silicon carbide monolithic materials, the synthesis steps are as follows: 1.5g SBA-15 monolithic Put it in a flask and vacuumize for 1.5 hours; Dissolve 2.0g PCAS in 18g xylene and stir magnetically for 2 hours; inject the xylene solution of PCAS into the flask and continue vacuuming for 0.5 hours; return to normal pressure and soak for 8 hours; The mixture was then put into an oven and kept at 80° C. for 10 hours; when filling for the second time, the amounts of polycarbosilane and xylene were 0.5 g and 3.5 g, respectively. Then the obtained dark brown solid was transferred to a muffle furnace and solidified at 220°C for 40 hours; finally, the obtained brown solid was put into a tube furnace and roasted in an argon atmosphere at 1200°C for 6 hours to obtain silicon carbide and Composite of silica. Soak the composite ...

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Abstract

The invention relates to a method for obtaining an ordered nano-mesoporous silicon carbide material by converting polycarbosilane with a high ceramic conversion ratio into silicon carbide in an in-situ manner. The silicon carbide material is prepared through the following steps: firstly, vacuumizing a template, and mixing a precursor solution with the template under vacuum conditions; stirring and carrying out heat treatment, so as to obtain a fulvous solid substance; curing a silicon carbide precursor in a certain curing cycle; roasting at a high temperature under the protection of inert gas, so as to enable the silicon carbide precursor to be pyrolyzed completely to obtain a compound of silicon carbide and silicon dioxide; finally, removing the template through a hydrofluoric acid solution, filtering, washing and drying, so as to obtain ordered nano-mesoporous silicon carbide material. The ordered nano-mesoporous silicon carbide material composed of purely chemical components and obtained through high temperature pyrolysis has relatively uniform hole diameters, is good in thermo oxidative stability, and is powdery or single piece-shaped.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and specifically relates to a kind of mesoporous silicon oxide as a template, high ceramic conversion rate polycarbosilane in-situ conversion, high stability and ordered mesoporous silicon carbide material and its preparation method. technical background [0002] Because of its high specific surface area, mesoporous materials have broad application prospects in many fields such as heterogeneous catalysts, adsorption separation, sensors, storage of natural gas and hydrogen, etc. Do your research. Mesoporous silicon carbide (SiC)-based ceramic materials have gradually entered people's field of vision because of their special structure and properties. SiC is a semiconductor and high-temperature ceramic with a wide band gap. It has strong Si-C covalent bonds in the lattice, so it has excellent properties of hardness and stability. At present, there are many methods for synthesizin...

Claims

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Application Information

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IPC IPC(8): C01B31/36
Inventor 周权王永丽倪礼忠张白雪
Owner EAST CHINA UNIV OF SCI & TECH
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