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Method for continuously preparing graphene powder in bulk

A graphene and powder technology, which is applied in the field of continuous large-scale preparation of powder graphene, can solve problems such as pollution, high oxygen content, and complicated post-processing, and achieve the effect of large application prospects, low oxygen content, and high quality

Active Publication Date: 2019-11-15
BEIJING GRAPHENE INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bottom-up growth method represented by chemical vapor deposition can realize the roll-to-roll growth of graphene film, and can obtain nearly 30 inches of graphene film (B.H.Hong, et al.Nat.Nanotech.2010,5,574 ), but the application of expensive metal catalysts and high energy consumption systems will inevitably limit the quantitative preparation of graphene films
The top-down exfoliation method represented by the Hummers method (W.S.Hummers, etal.J.Am.Chem.Soc.1958,80,1339) can realize the preparation of hundreds of tons of graphene powder at this stage, However, it is accompanied by problems such as poor quality of graphene, high oxygen content, complicated post-processing and serious pollution.
[0004] Therefore, how to prepare high-quality graphene in large quantities at low cost is still a huge challenge.

Method used

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  • Method for continuously preparing graphene powder in bulk
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  • Method for continuously preparing graphene powder in bulk

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Experimental program
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Effect test

preparation example Construction

[0040] The powder graphene continuous heavy-duty preparation method provided by the present invention is realized by a microwave plasma chemical vapor deposition system, comprising the following steps:

[0041] S1, feeding an inert gas into the microwave plasma chemical vapor deposition system to generate plasma;

[0042] S2, introducing a carbon source into the microwave plasma chemical vapor deposition system for vapor phase growth of powdered graphene;

[0043] S3, stop feeding the carbon source, and feed the etchant to etch the residual graphene in the microwave plasma chemical vapor deposition system; and

[0044] S4, repeat steps S1-S3, to realize the continuous large-scale preparation of powder graphene.

[0045] figure 1 It is a structural schematic diagram of the microwave plasma chemical vapor deposition system adopted in the present invention, as figure 1 As shown, the microwave plasma chemical vapor deposition system includes a short circuit 1 , a microwave reac...

Embodiment 1

[0062] use as figure 1 In the shown microwave plasma chemical vapor deposition system, 1200 sccm Ar is introduced to blow off the residual air in the system.

[0063] By adjusting the microwave power to 700W and initiating the system to generate Ar plasma, and then passing 3sccm CH 4 into the system. At this time, the system produces bright luminescence, and at the same time, black flocs can be seen continuously drifting away from the system at the end of the quartz tube, and the black flocs are collected.

[0064] After about 25 minutes of reaction, close the CH 4 Flowmeter, and it can be seen that there are many black substances remaining on the quartz tube wall in the microwave reaction chamber area. Under the power of 700W, 9.9sccm oxygen is introduced into the system at this time, and the black carbon substance can be seen to gradually decrease through the opening of the reaction chamber 2. After about 1 to 2 minutes, it can be seen that there is no obvious black subst...

Embodiment 2

[0073] use as figure 1 In the shown microwave plasma chemical vapor deposition system, 1200 sccm Ar is introduced to blow off the residual air in the system.

[0074] By adjusting the microwave power to 700W and initiating the system to generate Ar plasma, and then passing 3sccm CH 4 into the system. At this time, the system produces bright luminescence, and at the same time, black flocs can be seen continuously drifting away from the system at the end of the quartz tube, and the black flocs are collected.

[0075] After about 25 minutes of reaction, close the CH 4 Flowmeter, and it can be seen that there are many black substances remaining on the quartz tube wall in the microwave reaction chamber area. At this time, 9.9 sccm oxygen was introduced into the system, and after about 1 to 2 minutes, no obvious black substance remained on the quartz tube wall in the microwave reaction chamber area, indicating that the remaining graphene in this area was completely etched.

[00...

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Abstract

The invention provides a method for continuously preparing graphene powder in bulk. The method comprises the steps that S1, inert gas is introduced into a microwave plasma chemical vapor deposition system so as to generate plasmas; S2, a carbon source is introduced into the microwave plasma chemical vapor deposition system for the vapor phase growth of the graphene powder; S3, the carbon source stops from being introduced, an etching agent is introduced to etch graphene remaining in the microwave plasma chemical vapor deposition system; S4, the steps S1 to S3 are repeated, so that continuous in-bulk preparation of the graphene powder is achieved. By means of the method, long-time continuous preparation of the graphene powder can be achieved, the obtained graphene powder is high in quality,high in purity and low in oxygen content, and all the graphene powder is laminar graphene with the size lower than 300 nm, continuous in-bulk preparation of the graphene sheets is facilitated, and the method is great in application prospect.

Description

technical field [0001] The invention relates to the field of carbon materials, in particular to a method for continuously producing graphene powder in large quantities. Background technique [0002] In 2004, Professor Geim and Dr. Novoselov prepared single-layer graphene by tape stripping method (K.S. Novoselov, et al. Science 2004, 306, 666), and the two also won the 2010 Nobel Prize in Physics, which has triggered a There is a great research boom. Graphene has excellent properties, such as a large specific surface area, high Young's modulus and electron mobility, and the highest thermal conductivity, etc., making it have great application prospects in the fields of sensors, catalysis, and energy. [0003] The preparation of graphene mainly has two methods: bottom-up growth and top-down exfoliation. The bottom-up growth method represented by chemical vapor deposition can realize the roll-to-roll growth of graphene film, and can obtain nearly 30 inches of graphene film (B....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/186
CPCC01B2204/32C01B32/186
Inventor 张锦孙阳勇刘海舟高振飞许世臣
Owner BEIJING GRAPHENE INST
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