Preparation method of graphene

A technology of graphene and graphene solution, applied in the direction of graphene, nanotechnology for materials and surface science, nanocarbon, etc., can solve the problems of high and low specific surface area of ​​graphene, restricting the application of graphene, etc.

Inactive Publication Date: 2014-03-12
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods currently have some shortcomings, and the theoretical specific surface area of ​​graphene can reach 2630m 2 / g, but in fact the specific surface area of ​​prepared graphene is much lower than this value, most of them are only 600m 2 / g, which greatly restricts the application of graphene
And the yield of some obtained graphene is only about 10%
For example, graphene prepared by chemical vapor deposition has high specific surface area but low yield, and graphene prepared by redox method has high yield but low specific surface area.

Method used

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preparation example Construction

[0023] see figure 1 , the preparation method of the graphene of an embodiment comprises the following steps:

[0024] Step S101, dispersing graphite in ionic liquid to form a mixture of graphite and ionic liquid.

[0025] In this embodiment, graphite is preferably natural flake graphite, artificial graphite, amorphous carbon or expanded graphite. The ionic liquid is preferably 1-ethyl-3-methylimidazolium tetrafluoroboric acid (EtMeImBF 4 ), 1-ethyl-3-methylimidazole trifluoromethanesulfonimide (EtMeImN(CF 3 SO 2 ) 2 ), 1-ethyl-3-methylimidazole trifluoromethanesulfonic acid (EtMeImCF 3 SO 3 ), 1-ethyl-3-methylimidazole trifluoroacetic acid (EtMeImCF 3 CO 2 ), 1-ethyl-3-methylimidazole trifluoromethanesulfonyl carbon (EtMeImC(CF 3 SO 2 ) 3 ), 1-ethyl-3-methylimidazole pentafluoroacetimide (EtMeImN(C 2 f 5 SO 2 ) 2 ), 1-ethyl-3-methylimidazolium dicyanide nitrogen (EtMeImN(CN) 2 ), 1-ethyl-3,5-dimethylimidazolium trifluoromethanesulfonimide (1-Et-3,5-Me 2 ImN(CF...

Embodiment 1

[0036] A kind of preparation method of graphene, its technological process is as follows:

[0037] (1) Prepare 1L of a mixture of natural flake graphite and 1-ethyl-3-methylimidazolium tetrafluoroboric acid with a concentration of 1g / L of natural flake graphite.

[0038] (2) Put the prepared mixture in a 4L stainless steel ball mill container, add balls with a diameter of 5mm, the volume ratio of the added balls to the mixture is 1:2, that is, the volume of the balls is 2L, and then add The lid is sealed. A stainless steel ball milling vessel is installed in the ball milling equipment, the ball milling speed is set at 200 rpm, and the equipment is stopped after 12 hours of ball milling to obtain a slurry.

[0039] (3) Take out the ball milling container, separate the ball milling balls from the solution with a sieve, and centrifuge at a speed of 1000 rpm for 10 minutes with a centrifuge to separate the unexfoliated graphite to obtain a graphene solution.

[0040] (4) Filter th...

Embodiment 2

[0043] A kind of preparation method of graphene, its technological process is as follows:

[0044] (1) Prepare 1L of a mixture of artificial graphite and 1-ethyl-3-methylimidazolium trifluoromethanesulfonimide with an artificial graphite concentration of 10g / L.

[0045] (2) Put the prepared mixture in a 4L stainless steel ball mill container, add balls with a diameter of 10mm, the volume ratio of the added balls to the mixture is 1:1, that is, the volume of the balls is 1L, and then add The lid is sealed. The stainless steel ball milling container is installed in the ball milling equipment, the ball milling speed is set at 400 rpm, and the equipment is stopped after 10 hours of ball milling to obtain the slurry.

[0046] (3) Take out the ball milling container, separate the ball milling balls from the solution with a screen, and centrifuge at a speed of 2000 rpm for 5 minutes to separate the unexfoliated graphite to obtain a graphene solution.

[0047] (4) Filter the graphen...

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Abstract

A preparation method of graphene comprises the steps of: dispersing the graphite in an ionic liquid to form a mixture of graphite and ionic liquid; placing the mixture of graphite and ionic liquid in a ball-milling container, adding milling balls to carry out ball-milling, so as to obtain a slurry; taking the slurry out of the ball-milling container, separating the milling balls and conducting centrifugation and separation to obtain a graphene solution; and carrying out filtering, washing and drying treatment on the graphene solution to obtain the graphene. The ball milling method uses the ion liquid as a solvent to prepare the graphene with good dispersion, effectively prevents re-agglomeration of the graphite, and realizes large reaction amount, high yield and high specific surface area of the obtained graphene.

Description

technical field [0001] The invention relates to the technical field of organic semiconductor materials, in particular to a preparation method of graphene. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004, and won the Nobel Prize in Physics in 2010, which once again sparked an upsurge in carbon material research. Due to its unique structure and photoelectric properties, it has become a research hotspot in the fields of carbon materials, nanotechnology, condensed matter physics and functional materials, attracting many scientific and technological workers. Single-layer graphene has excellent electrical and thermal conductivity and low thermal expansion coefficient, and its theoretical specific surface area is as high as 2630m2 / g (A Peigney, Ch Laurent, et al. Carbon, 2001, 39, 507), which can be used for effect transistors, electrode materials , composite materials, liquid cryst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y30/00C01B32/19
Inventor 周明杰王要兵袁新生钟辉
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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