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Method for preparing carbon materials rich in nano diamond structure

A nano-diamond and carbon material technology, applied in the direction of diamond, nanotechnology, carbide, etc., can solve the problems of nano-diamond quality influence, difficulty in large-scale promotion and application, slow synthesis rate, etc., to achieve high quality, low cost, and high synthesis speed fast effect

Inactive Publication Date: 2012-07-18
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there will be a lot of metal impurities in the nano-diamond synthesized by the traditional detonation method. These impurities have a great impact on the quality of the nano-diamond, and it is difficult to further purify it. It is possible to prepare relatively pure nano-diamonds, but due to the high cost of lasers and intense pulsed electron beam equipment and the slow synthesis rate, it is difficult to apply them on a large scale

Method used

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  • Method for preparing carbon materials rich in nano diamond structure
  • Method for preparing carbon materials rich in nano diamond structure
  • Method for preparing carbon materials rich in nano diamond structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 20g of titanium carbide powder with a particle size of 800 mesh, put it into a high-energy ball mill, and then put 80g of GCr15 bearing steel balls into it. In order to prevent the titanium carbide powder from agglomerating during the ball mill, put 1ml of ethanol as a dispersant. The speed of the ball mill is 220 rpm, ball milling time is 5 hours. At this time, the particle size of the titanium carbide powder was about 2.0 μm. Then put the titanium carbide powder obtained after the above ball milling into a fused silica tube furnace, vacuumize to 0.1 Pa, and then pass in argon gas. The temperature of the tube furnace was raised to 900° C., and chlorine gas was introduced at a flow rate of 30 ml / min for 2 hours. After the reaction is completed, argon gas is introduced to remove residual chloride on the surface of the titanium carbide powder, and after cooling to room temperature with the furnace, a carbon material rich in nano-diamond structure can be obtained.

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Embodiment 2

[0018] Take 20g of titanium carbide powder with a particle size of 800 mesh, put it into a high-energy ball mill, and then put 120g of GCr15 bearing steel balls into it. In order to prevent the titanium carbide powder from agglomerating during the ball mill, put 1ml of ethanol as a dispersant. The speed of the ball mill is 180 rpm, ball milling time is 20 hours. At this time, the particle size of the titanium carbide powder was about 0.5 μm. Then put the titanium carbide powder obtained after the ball milling into a fused silica tube furnace, vacuumize to 1 Pa, and then pass in argon gas. The temperature of the tube furnace was raised to 1200° C., and chlorine gas was introduced at a flow rate of 20 ml / min for 1 hour. After the reaction, argon gas is introduced to remove residual chloride on the surface of the titanium carbide powder. After cooling down to room temperature with the furnace, the carbon material rich in nano-diamond structure can be obtained.

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Embodiment 3

[0021] Take 20g of titanium carbide powder with a particle size of 800 mesh, put it into a high-energy ball mill, and then put 100g of GCr15 bearing steel balls into it. In order to prevent the titanium carbide powder from agglomerating during the ball mill, put 1ml of ethanol as a dispersant, and the speed of the ball mill is 200 rpm, ball milling time is 15 hours. At this time, the particle size of the titanium carbide powder was about 0.9 μm. Then put the titanium carbide powder obtained after the above ball milling into a fused silica tube furnace, vacuumize to 0.05 Pa, and then pass in argon gas. The temperature of the tube furnace was raised to 1100° C., and chlorine gas was introduced at a flow rate of 25 ml / min for 1.5 hours. After the reaction, argon gas is introduced to remove residual chloride on the surface of the titanium carbide powder. After cooling down to room temperature with the furnace, the carbon material rich in nano-diamond structure can be obtained.

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Abstract

The invention relates to a method for preparing carbon materials rich in a nano diamond structure, which comprises the following steps: firstly, placing titanium carbide powder into a high-energy ball mill to carry out ball milling pretreatment, wherein in the ball milling process, the ratio of ball to powder is 4:1 to 6:1, the rotating speed of the ball mill is 180 to 220 revolutions per minute, the ball milling time is 5 to 20 hours and the titanium carbide powder is ground and refined to have the particle size of 0.5 to 2.0mum; and then, placing the titanium carbide powder subjected to ball milling into a fused quartz tube furnace, filling argon after vacuumizing to the pressure of 0.05 to 1Pa, heating the tube furnace to 900 to 1,200 DEG C, filling chlorine gas at a flow velocity of 20 to 30ml / min, carrying out chlorination for 1 to 2 hours, filling the argon again after the reaction is finished, and cooling to the room temperature along with the furnace. The method has the advantages that the method has simple synthesis process and high efficiency; and a great amount of carbon materials rich in nano diamond with the particle size of 5 to 10 nanometers can be prepared.

Description

technical field [0001] The invention relates to the field of novel carbon materials, in particular to a method for preparing carbon materials. Background technique [0002] Nanodiamond has broad application prospects in many important fields due to its excellent properties such as extremely high hardness and compressive strength, excellent optical properties, and better biocompatibility. Therefore, the research and development of nanodiamond preparation technology and methods has always been concerned. [0003] So far, people have developed a variety of methods for preparing nano-diamonds, mainly including: (1) Explosive detonation synthesis method: it is to compress graphite into diamond during the detonation process of explosives. This is the traditional method of using explosives detonation The method of synthesizing nano-diamond; (2) laser bombardment synthesis method: carbon powder is transformed into diamond by high-speed laser bombardment, and Sun Jing et al. synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/06B82Y40/00C01B32/26C01B32/921
Inventor 张瑞军徐江周海朝王建新陈鹏
Owner YANSHAN UNIV
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