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Ball milling preparation method of graphene

A graphene and ball milling technology, which is applied in the field of preparing graphene materials, can solve the problems of many oxygen-containing functional group defects, cannot be mass-produced, and harsh conditions, and achieve the effect of simple equipment, convenient operation, and mild conditions

Inactive Publication Date: 2013-12-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to address the defects of the oxygen-containing functional groups on the surface of graphene prepared by the prior art, the harsh conditions or high cost, and the shortcomings that cannot be produced in large quantities. A preparation method of graphene material with low cost, high yield and simple and easy operation

Method used

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  • Ball milling preparation method of graphene

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Effect test

example 1

[0022] 1g of graphite powder, 5ml of naphthol polyoxyethylene ether, and 10ml of deionized water are mixed for ball milling. The diameter of the ball milling tank is 15cm, and the ball milling beads are mixed with a diameter of 6mm and 11mm. Fix it in a planetary ball mill with a rotating speed of 400rmp, and ball mill for 12h. The resulting product was transferred to 200ml deionized water, centrifuged at a speed of 3000rmp for 20min, and the upper layer solution was taken, which was dark black.

[0023] Graphene aqueous solution is vacuum filtered to prepare graphene film. The resistivity of the graphene film that has not been washed with ethanol is as high as 7 kohms per square, while the resistivity of the graphene film washed with ethanol is as low as 0.3 thousand ohms per square , indicating that the oxygen-containing functional group defects on the surface of graphene prepared by the present invention are few.

[0024] Such as figure 1 , Figure a is the graphene washed...

example 2

[0026] 1g of flake graphite, 2ml of naphthol polyoxyethylene ether, and 10ml of deionized water are mixed for ball milling. The diameter of the ball milling tank is 15cm, and the ball milling beads are mixed with a diameter of 6mm and 11mm. Fix it in a planetary ball mill with a rotating speed of 500rmp and ball mill for 10h. The resulting product was transferred to 200ml deionized water, centrifuged at a speed of 5000rmp for 20min, and the upper layer solution was taken, which was black. The resistivity of the graphene film that has not been washed with ethanol prepared by the method of Example 1 is as high as 5 thousand ohms per square, while the resistivity of the graphene film washed with ethanol is as low as 0.4 thousand ohms per square

example 3

[0028] 1g of pyrolytic graphite, 5ml of naphthol polyoxyethylene ether and 5ml of nonylnaphthol polyoxyethylene ether, and 10ml of deionized water are mixed for ball milling. The diameter of the ball milling tank is 15cm, and the diameter of the ball milling beads is 6mm and 11mm. Fix it on a planetary ball mill with a rotating speed of 500rmp and ball mill for 5h. The resulting product was transferred to 200ml deionized water, centrifuged at a speed of 8000rmp for 20min, and the upper layer solution was taken, which was slightly black. The resistivity of the graphene film that has not been washed with ethanol prepared by the method of Example 1 is as high as 10 kilohm per square, while the resistivity of the graphene film washed with ethanol is as low as 0.2 thousand ohm per square.

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Abstract

The invention provides a ball milling preparation method of graphene. The ball milling preparation method comprises the following steps of: putting a mixture of graphite carbon and an alkyl six-membered aromatic ring or condensed ring polyether nonionic surfactant in the mass-volume ratio of 1: 2 to 1: 15, and deionized water in a ball milling jar, and fixing the ball milling jar on a ball mill for ball milling at a rotating speed ranging from 200 to 500 rpm for 5-30 hours; next, transferring the ball milled mixture to deionized water for centrifuging at a rotating speed ranging from 3000 to 8000 rpm for 10-30 minutes, and then obtaining a black upper-layer colloidal suspension for preparing graphene aqueous solutions with different concentrations. The graphene produced by the ball milling preparation method provided by the invention is dispersed in aqueous solutions and is high in concentration; the surfactant can be easily removed by using ethanol, which is friendly to environment and advantageous for wide application of graphene. The adopted ball milling equipment is simple, convenient to operate and safe to run; no new surface oxygen-containing functional group defect is introduced by ball milling; furthermore, the ball milling preparation method is mild and simple in preparation process, and high in yield.

Description

technical field [0001] The invention relates to a method for preparing graphene materials related to the technical field of nanometer materials, in particular to a method for obtaining graphene materials in a new processing manner. Background technique [0002] Graphene is a two-dimensional atomic crystal material composed of a single layer of closely arranged carbon atoms. In 2004, the graphite monolithic sheet was obtained by the scientist Geim A K et al. by repeatedly peeling off the graphite sheet through tape. Before the discovery of graphene, it was believed theoretically and experimentally that the perfect two-dimensional structure could not exist stably at non-absolute zero temperature, so the discovery of graphene attracted the attention of the whole world, and its discoverer won the Nobel Prize in 2010 Physics Prize. [0003] In fact, graphene is the building block of carbon-based materials in other dimensions. Zero-dimensional fullerenes can be regarde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 刘洪涛毛敏
Owner CENT SOUTH UNIV
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