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Method for regulating pore structure of carbide derived carbon

A carbide-derived carbon and pore structure technology, which is applied in the preparation/purification of carbon, can solve the problems of material specific surface reduction and reduction, and achieve the effects of sharp reduction of specific surface, simple process, and simple reaction equipment

Inactive Publication Date: 2012-11-21
YANSHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The research by Alar J?nes et al. found that changing the chlorination reaction temperature of carbides can effectively control the pore structure of the obtained carbide-derived carbons, but the appearance of mesopores under high temperature conditions caused a sharp decrease in the specific surface of the material.
Jaan Leis et al. mixed iron-group catalysts when titanium carbide was chlorinated. As a result, a large number of mesopores appeared in the obtained CDC, but the specific surface of the material decreased sharply.
Although the above methods have a good control effect on the pore structure of carbide-derived carbon, there is a phenomenon that the specific surface area decreases sharply when the mesopore structure appears.

Method used

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  • Method for regulating pore structure of carbide derived carbon
  • Method for regulating pore structure of carbide derived carbon
  • Method for regulating pore structure of carbide derived carbon

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Take 20g of titanium carbide powder with a particle size of 800 mesh and put it into a high-energy ball mill, put in 120g of GCr15 bearing steel balls, and then put in 1ml of ethanol as a dispersant. The speed of the ball mill is 280 rpm, and the ball milling time is 8 hours. At this time, the particle size of the titanium carbide powder was about 1.2 μm. Then put the above-mentioned titanium carbide powder into a fused silica tube furnace, vacuumize to 0.1Pa and then pass in argon gas, raise the temperature of the tube furnace to 600°C, and pass in chlorine gas at a flow rate of 20ml / min for 3.0 Hour. After the reaction is completed, argon gas is introduced to remove residual chloride on the surface of the titanium carbide powder, and after the temperature is cooled to room temperature, a high specific surface carbide-derived carbon with a mesopore structure is obtained.

[0014] Such as figure 1 As shown, under the same process and parameters of the high-temperature...

Embodiment 2

[0016] Take 20g of titanium carbide powder with a particle size of 800 mesh and put it into a high-energy ball mill, put in 160g of GCr15 bearing steel balls, and then put in 1ml of ethanol as a dispersant. The speed of the ball mill is 240 rpm, and the ball milling time is 12 hours. At this time, the particle size of the titanium carbide powder was about 0.6 μm. Then put the above-mentioned titanium carbide powder into a fused silica tube furnace, vacuumize to 0.05Pa, and then pass in argon gas. The temperature of the tube furnace was raised to 800° C., and chlorine gas was introduced at a flow rate of 30 ml / min for 1.0 hour. After the reaction is completed, argon is introduced to remove residual chloride on the surface of the titanium carbide powder. After the temperature drops to room temperature, a high specific surface carbide-derived carbon with a mesopore structure can be obtained.

[0017] Such as figure 2 As shown, under the same process and parameters of the high...

Embodiment 3

[0019] Take 20g of titanium carbide powder with a particle size of 800 mesh and put it into a high-energy ball mill, put in 140g of GCr15 bearing steel balls, and then put in 1ml of ethanol as a dispersant. The speed of the ball mill is 260 rpm, and the ball milling time is 10 hours. At this time, the particle size of the titanium carbide powder was about 0.9 μm. Then put the above-mentioned titanium carbide powder into a fused silica tube furnace, evacuate to 1 Pa, and then pass in argon gas. The temperature of the tube furnace was raised to 1000° C., and chlorine gas was introduced at a flow rate of 25 ml / min for 2.0 hours. After the reaction is completed, argon is introduced to remove residual chloride on the surface of the titanium carbide powder. After the temperature drops to room temperature, a high specific surface carbide-derived carbon with a mesopore structure can be obtained.

[0020] Such as image 3 As shown, under the same process and parameters of the high-te...

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Abstract

A method for regulating a pore structure of carbide derived carbon (CDC). The method comprises the following steps of: putting titanium carbide powder into a high-energy ball mill in the ball-material ratio of 6-8 : 1 at a rotating speed of 240-280 revolutions per minute for 8-12 hours, and smashing and refining the particle size of the titanium carbide powder to 0.6-1.2 [mu]m; and putting the ball-milled titanium carbide powder into a melting quartz tubular furnace, vacuumizing to 0.05-1Pa, introducing argon gas, heating the tubular furnace to 600-1000 DEG C, introducing chlorine gas at a flow speed of 20-30 ml / min for 1-3 hours, introducing argon gas once again after a reaction, removing chlorides such as titanium tetrachloride and the like left on the surface of the titanium carbide powder under the scouring effect of the argon gas flow, and cooling to the room temperature. The method has the advantages of simple and convenient process, simple reaction equipment and capability of effectively controlling the pore structure of CDC and resolving the problems of sharply reduced specific surface when mesoporous appearances.

Description

technical field [0001] The invention belongs to the field of novel carbon materials, in particular to a preparation method of porous carbon materials. Background technique [0002] Carbide-derived carbon (CDC) is a new type of porous carbon material. It is formed by taking away non-carbon atoms in carbides in the form of gas halides under high temperature conditions. Studies have shown that the high specific surface area and controllable pore structure of CDC make it a great potential for application in fields such as hydrogen storage, catalyst supports, molecular sieves, and supercapacitors. [0003] At present, there are several methods to regulate the pore structure of CDC: (1) changing the chlorination reaction temperature; (2) adding catalyst; (3) changing the reaction precursor, etc. The research by Alar J?nes et al. found that changing the chlorination reaction temperature of carbides can effectively control the pore structure of the obtained carbide-derived carbons...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 张瑞军徐江周海朝王建新陈鹏
Owner YANSHAN UNIV
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