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Method for preparing porous nano-silicon carbide by using silicate glass as raw material

A technology of nano-silicon carbide and silicate glass, which is applied in chemical instruments and methods, nanotechnology for materials and surface science, carbon compounds, etc., and can solve the problems of difficult to obtain porous structure, harsh reaction conditions, and high cost. , to achieve considerable economic effects, safe reaction, and full response

Active Publication Date: 2017-12-01
WUHAN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] In view of the above defects or improvement needs of the prior art, the present invention provides a method for preparing porous nano-silicon carbide using silicate-based glass as a raw material. The purpose is to use silicate glass powder as raw material and coal tar as carbon Source, using magnesium halide as molten salt, reacting in the molten state of glass, and finally preparing nano-porous silicon carbide by pickling, thus solving the problem of harsh reaction conditions, high cost, and porous structure in the prior art nano- and porous silicon carbide preparation methods Technical problems such as difficulty in obtaining or unstable structure

Method used

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  • Method for preparing porous nano-silicon carbide by using silicate glass as raw material
  • Method for preparing porous nano-silicon carbide by using silicate glass as raw material
  • Method for preparing porous nano-silicon carbide by using silicate glass as raw material

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preparation example Construction

[0038] The preparation method of the nano-silicon carbide is as follows: mix silicate glass, magnesium powder, carbon source and molten salt, and heat it to 600-750°C for 1-12 hours at a heating rate of 1-30°C / min under an inert atmosphere. After the product is cooled to room temperature with the furnace, it is acid-washed to obtain nano-silicon carbide.

[0039] Among them, the silicate glass is sodium silicate glass or calcium silicate glass; the molten salt is magnesium halide, including magnesium chloride, magnesium bromide or magnesium iodide, preferably magnesium chloride; coal tar is selected as the carbon source; silicate glass, magnesium powder , the molten salt and the carbon source are mixed according to a mass ratio of 1:(0.5-0.8):(5-8):(0.5-2).

[0040] Specifically, the preparation method includes the following steps:

[0041] (1) mechanically ball-milling the silicate glass into glass powder after cleaning to obtain powdered silicate glass;

[0042] (2) Mix th...

Embodiment 1

[0058] A preparation method for preparing porous nano-silicon carbide using silicate-based glass as a raw material is carried out according to the following steps:

[0059] (1) 5g silicate glass is mechanically ball-milled into powder after cleaning;

[0060] (2) Ball milled silicate glass powder, magnesium powder, molten salt (MgCl 2 ), coal tar is ball milled and mixed evenly according to the mass ratio of 1:0.6:8:1;

[0061] (3) Then put the mixture into a tube furnace and heat it to 650° C. for 3 hours at a heating rate of 5° C. / min. After the product is cooled to room temperature with the furnace, take it out;

[0062] (4) The obtained product was first washed in 1 mol / L hydrochloric acid for 1 hour, then washed in hydrofluoric acid with a mass fraction of 5% for 3 hours, filtered by suction and dried to obtain porous silicon carbide nanoparticles.

[0063] Characterization and analysis of the prepared porous nano-silicon carbide particles:

[0064] Depend on figure 1...

Embodiment 2

[0068] A preparation method for preparing porous nano-silicon carbide using silicate-based glass as a raw material is carried out according to the following steps:

[0069] (1) 5g silicate glass is mechanically ball-milled into powder after cleaning;

[0070] (2) Ball milled silicate glass powder, magnesium powder, molten salt (MgCl 2 ), coal tar is ball milled and mixed evenly according to the mass ratio of 1:0.6:7:1;

[0071] (3) Then put the mixture into a tube furnace and heat it to 600°C for 12 hours at a heating rate of 1°C / min, and take it out after the product is cooled to room temperature with the furnace;

[0072] The obtained product was first washed in 1 mol / L hydrochloric acid for 1 hour, then washed in hydrofluoric acid with a mass fraction of 5% for 3 hours, filtered by suction and dried to obtain porous silicon carbide nanoparticles.

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Abstract

The invention discloses a method for preparing nano-silicon carbide by using silicate-based glass as a raw material. The method comprises the following steps: carrying out mechanical ball milling on glass; carrying out uniform ball milling and mixing on the ball-milled powdery glass, magnesium powder, coal tar and molten salt according to a certain proportion, and placing into a container for reaction under inert gas; then pickling the reaction product to obtain nano-silicon carbide. The method disclosed by the invention has the advantages that steps are simple and easy and the source of raw materials is wide; further, the Mg-containing molten salt is added as a heat absorbent to control the reaction temperature and increase the solubility and wettability of magnesium so as to enable the reaction to be more sufficient and the reactants not to agglomerate easily. The three-dimensional porous silicon carbide prepared by the method has the advantages of relatively high purity, uniform particle, high specific surface area (180-260m<2> / g), rich mesoporous structure and the like, and has wide application prospects in the aspects of radiation resistance, radiation resistance and wave absorption.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and more specifically relates to a method for preparing porous nanometer silicon carbide using silicate-based glass as a raw material. Background technique [0002] Nano-silicon carbide materials have high band gap, high critical breakdown electric field and thermal conductivity, small dielectric constant and high electron saturation mobility, as well as strong radiation resistance and good mechanical properties. Ideal materials for electronic and optoelectronic devices with high frequency, high power, low energy consumption, high temperature resistance and radiation resistance, it is generally believed that it is expected to become an important component unit of the third-generation wide bandgap semiconductor materials. [0003] At present, the preparation methods of nano silicon carbide include ball milling method, plasma method and carbothermal reduction method. The ball milling method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/963B82Y30/00
Inventor 霍开富高标安威力梅世雄付继江张旭明
Owner WUHAN UNIV OF SCI & TECH
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