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Method for preparing graphene by peeling off graphite

A technology for exfoliating graphite and graphene, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, and can solve problems such as expensive, cost-increasing, and low production efficiency

Active Publication Date: 2014-11-26
TORAY IND INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the biggest disadvantage of this method is that only a small amount of graphene can be obtained, and the production efficiency is extremely low.
Chinese patent CN201210249137.1 prepares graphene by mechanically grinding graphite in ionic liquid. The disadvantage of this method is that expensive ionic liquid is used as a solvent
The addition of ultrasound will increase the entire preparation process steps a lot, and the cost will increase a lot. What is more troublesome is that the local high temperature and high pressure caused by the cavitation effect of ultrasound will destroy the graphene crystal and bring many structural defects to graphene.

Method used

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  • Method for preparing graphene by peeling off graphite
  • Method for preparing graphene by peeling off graphite
  • Method for preparing graphene by peeling off graphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Pour 0.5 grams of 50-mesh expanded graphite into a zirconia ball mill jar with a volume of 100 milliliters, then add 18 milliliters of 98.5% concentrated sulfuric acid, and finally add 100 diameters of 5 mm, 30 diameters of 7 mm, and 4 diameters of 10 mm zirconia grinding balls (the total weight of the three kinds of grinding balls is 81 grams), cover the ball grinding tank, and then seal the tank with PARA film. The above-mentioned sealed ball mill jar was placed on a planetary ball mill and ball milled at a speed of 500 rpm for 20 hours. Pour all the black mixture in the tank into 400 ml of deionized water, separate the balls inside to obtain a black slurry, add water and centrifuge until the pH of the product is greater than 6 (indicating that there is basically no residual acid), and finally dry, That is, a graphene powder product is obtained.

[0028] The scanning electron micrograph of the resulting graphene is shown in figure 2 with image 3 . from figure ...

Embodiment 2

[0030] Pour 0.5 grams of 325-mesh expanded graphite into a zirconia ball mill jar with a volume of 100 milliliters, then add 18 milliliters of 98.5% concentrated sulfuric acid, and finally add 100 diameters of 5 mm, 30 diameters of 7 mm, and 4 diameters of 10 mm zirconia grinding balls (the total weight of the three kinds of grinding balls is 81 grams), cover the ball grinding tank, and then seal the tank with PARA film. The above-mentioned sealed ball mill jar was placed on a planetary ball mill and ball milled at a speed of 500 rpm for 20 hours. Pour all the black mixture in the tank into 400 ml of deionized water, separate the grinding balls inside to obtain a black slurry, filter and wash by adding water until the pH value of the product is greater than 6 (indicating that there is basically no residual acid), and finally dry, That is, a graphene powder product is obtained. The powder resistivity and film resistivity of the obtained product are listed in Table 1.

Embodiment 3

[0032] Pour 0.5 grams of 325-mesh expanded graphite into a zirconia ball mill jar with a volume of 100 milliliters, then add 27.5 milliliters of 98.5% concentrated sulfuric acid, and finally add 120 diameters of 5 mm, 40 diameters of 7 mm, and 4 diameters of 10 mm zirconia grinding balls (the total weight of the three kinds of grinding balls is 100 grams), cover the ball grinding tank, and then seal the tank with PARA film. The above-mentioned sealed ball mill jar was placed on a planetary ball mill and ball milled at a speed of 500 rpm for 6 hours. Pour all the black mixture in the tank into 400 ml of deionized water, separate the balls inside to obtain a black slurry, add water and centrifuge until the pH of the product is greater than 6 (indicating that there is basically no residual acid), and finally dry, That is, a graphene powder product is obtained. The powder resistivity and film resistivity of the obtained product are listed in Table 1.

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Abstract

The invention provides a process method for preparing graphene by peeling off graphite. The method comprises the following steps: putting the graphite, a grinding material and concentrated sulfuric acid into grinding equipment, and grinding the materials to obtain a mixture; and separating the sulfuric acid and the grinding material out of the mixture, and washing and drying the remaining materials to obtain the graphene. The preparation flow of the graphene is very short, the cost is low, and the prepared graphene is complete in crystal form, has high conductivity, ad can be widely applied to a plurality of fields of battery materials, composite materials, electronic devices, energy storing materials and the like.

Description

technical field [0001] The invention belongs to the technical field of nano-carbon materials, and in particular relates to a preparation method of graphene. Background technique [0002] Due to its excellent mechanical, electrical, thermal and optical properties, graphene has broad application prospects in many fields such as battery materials, composite materials, electronic devices and energy storage materials. Therefore, the preparation of graphene has always been the focus of attention. The preparation methods that have been reported so far mainly include mechanical exfoliation method, epitaxial growth method, chemical vapor deposition method and redox method. Although epitaxial growth and vapor deposition can produce high-quality graphene, the equipment investment is large, the process is complicated, and the cost is high. Although the oxidation-reduction method can prepare graphene in large quantities and cheaply, the disadvantage is that the oxidized graphite cannot...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y30/00
Inventor 刘刚桥孙培育吴祯琪
Owner TORAY IND INC
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