Graphene and preparation method thereof

A graphene and graphite rod technology, applied in the field of electrochemistry, can solve problems such as higher requirements for production equipment, limitation of graphene performance, human body and environmental hazards, etc., to achieve easy large-scale industrial production, realize large-scale industrial production, improve energy storage effect

Active Publication Date: 2014-08-06
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Abstract
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AI Technical Summary

Problems solved by technology

At present, the methods for preparing graphene mainly include mechanical exfoliation method, epitaxial growth method, redox method and chemical vapor deposition method, and the amount of graphene prepared by mechanical exfoliation method and epitaxial growth method is low, and the thickness is not uniform; redox method It is mainly divided into oxidative thermal reduction and oxidative chemical reduction. The preparation of graphene by oxidative thermal reduction often requires higher temperature and consumes a lot of energy, while the preparation of graphene by chemical reduction often uses chemical reagents such as hydrazine. These reagents have certain toxicity. Harmful to the human body and the environment; graphene is prepared by chemical vapor deposition, which requires high production equipment
[0003] The theoretical specific surface area of ​​graphene is relatively high, which can reach 2630m 2 / g, but in fact the specific surface area is relatively low, basically at 500m 2 Below / g, this limits many properties of graphene, such as energy storage performance, etc.

Method used

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  • Graphene and preparation method thereof

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preparation example Construction

[0016] The preparation process of graphene of the present invention is roughly divided into the following steps:

[0017] 1. Take graphite with a purity of 99.5% to make a graphite rod, use the graphite rod as the positive electrode and the platinum rod as the negative electrode, and connect them to the two poles of the external power supply respectively, so as to apply an external voltage to the positive and negative electrodes in the subsequent steps;

[0018] 2. Then insert the positive graphite rod and the negative platinum rod into the electrolyte solution, apply a small voltage of 0.8V~1.5V between the positive and negative electrodes, keep it for 1~5 minutes and stop, and then apply 10V~15V between the positive and negative electrodes. High voltage and keep it for 4~15 minutes to stop, then filter the electrolyte solution and dry it;

[0019] The purpose of this step is to use the principle of chemical intercalation, first apply a small voltage to lightly intercalate gr...

Embodiment 1

[0026] The preparation steps of graphene in the present embodiment are as follows:

[0027] 1. Graphite rods with a purity of 99.5% are made of graphite rods, and the graphite rods are used as positive electrodes and platinum rods as negative electrodes, which are respectively connected to the two poles of the external power supply;

[0028] 2. Insert the positive and negative electrodes into the electrolyte. The electrolyte is mixed with 1 g of deionized water and 1 g of 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt. A voltage of 1.2V was applied between the positive and negative electrodes for 5 minutes, and then a voltage of 10V was applied between the positive and negative electrodes for 5 minutes. After 5 minutes, the electrolyte solution was filtered, and the solid product was placed in a vacuum oven at 60°C for 48 hours. Vacuum dry for 12 hours.

[0029] 3. Put the dried solid product in an argon atmosphere with a flow rate of 400ml / min, and use 4×10 1...

Embodiment 2

[0032] The preparation steps of graphene in the present embodiment are as follows:

[0033] 1. Graphite rods with a purity of 99.5% are made of graphite rods, with graphite rods as positive electrodes and platinum rods as negative electrodes, respectively connected to the two poles of the external power supply, so as to apply external voltages to the positive and negative electrodes in subsequent steps;

[0034] 2. Insert the positive and negative electrodes into the electrolyte mixed with 2g of deionized water and 1g of 1-ethyl-3-methylimidazole bis-trifluoromethanesulfonimide salt, and apply a voltage of 1V between the positive and negative electrodes for a continuous period of time. 4 minutes, then apply 12V voltage between positive and negative electrodes, after lasting 4 minutes, the electrolyte solution is filtered, and the solid product is placed in the vacuum oven of 100 ° C for 24 hours;

[0035] 3. Put the dried solid product under the protection of argon with flow r...

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Abstract

The present invention relates to graphene and a preparation method thereof. The preparation method comprises: adopting a graphite rod as a positive electrode, adopting a platinum rod as a negative electrode, and connecting into an external power supply; inserting the positive electrode and the negative electrode into an electrolyte solution, applying a voltage of 0.8-1.5 V, maintaining for 1-5 min, stopping, applying a voltage of 10-15 V, maintaining for 4-15 min, and filtering and drying the electrolyte solution; and placing the dried solid product in an inert gas atmosphere, and adopting laser with a frequency of 4*10<14>-7.5*10<14> HZ to irradiate to obtain the graphene. According to the present invention, the electrochemical intercalation method and the laser stripping method are adopted to efficiently convert graphite into graphene, such that the prepared graphene has extremely high specific surface area so as to improve the energy storage property and the like of the graphene; and the equipment and the process required during the preparation process are simple and are easy to operate, the raw materials are cheap, the cost is low, and large-scale industrial production is easily achieved.

Description

technical field [0001] The invention relates to the field of electrochemistry, in particular to a graphene and a preparation method thereof. Background technique [0002] Graphene is a two-dimensional monolayer material with excellent physical properties, such as high theoretical specific surface area, excellent mechanical strength, good flexibility and high electrical conductivity, etc., so it has received extensive attention from researchers. . At present, the methods for preparing graphene mainly include mechanical exfoliation method, epitaxial growth method, redox method and chemical vapor deposition method, while the amount of graphene prepared by mechanical exfoliation method and epitaxial growth method is relatively low, and the thickness is not uniform; redox method It is mainly divided into oxidative thermal reduction and oxidative chemical reduction. The preparation of graphene by oxidation thermal reduction often requires higher temperature and consumes a lot of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/16
Inventor 周明杰钟辉王要兵刘大喜
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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