Process for preparing graphene by cryochemical method

A low-temperature chemistry and graphene technology, which is applied in the low-temperature catalytic reduction preparation of graphite nanomaterials and the low-temperature chemical method for graphene preparation, can solve the problems of severe reduction reaction, incomplete reduction, and high reaction activity, and achieves low reduction temperature and reduced reduction. Simple method, mild reaction and controllable effect

Active Publication Date: 2013-08-21
TSINGHUA UNIV
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Problems solved by technology

Based on these studies, it can be found that the step of graphene oxide reduction is the key to the preparation of graphene by chemical redox method, and the existing reducing agent reduction method has the problem of incomplete reduction.
In addition, the organic reducing agent hydrazine and its derivatives are highly toxic and not an environmentally friendly reducing agent
However, the reactivity of sodium hydride and the like is too high, causing the reduction reaction to be too violent and difficult to control

Method used

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  • Process for preparing graphene by cryochemical method

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preparation example Construction

[0023] The preparation method of graphene oxide used in the example: mix 3g of graphite powder, 3g of sodium nitrate and 138ml of concentrated sulfuric acid in an ice bath; then slowly add 18g of potassium permanganate, magnetically stir and mix, and then heat in a 35°C water bath for 1h; Then add 240ml of deionized water and heat at 90°C for 0.5h. After the heating, add 600ml of deionized water and 18ml of hydrogen peroxide.

[0024] The reduced graphene is prepared into a graphene film by means of suction filtration, and then the film thickness of the graphene film is measured by a step meter, and its electrical conductivity is measured by a four-probe method.

Embodiment 1

[0026] 120 mg of graphene oxide (GO) was dispersed in 200 ml of N,N-dimethylformamide (DMF), 1 g of sodium borohydride was dissolved in 25 ml of DMF, and 0.07 g of anhydrous aluminum chloride was dissolved in 25 ml of DMF. Then the three solutions were mixed and reduced at 140 °C for 3 h under magnetic stirring.

[0027] The test result is: the conductivity of the graphene film is 820S / m.

[0028] Under the catalytic conditions of different catalysts, the reduction temperature and reduction time are changed, and other conditions remain unchanged, the conductivity of other graphene obtained is shown in the following table:

[0029]

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Abstract

The invention discloses a process for preparing graphene by a cryochemical method, belonging to the technical field of chemical synthesis of graphene. The process uses graphene oxide prepared by chemical oxidation as a raw material, and comprises the step of reducing reaction in which graphene oxide is reduced into graphene. The reducing reaction step implements reduction of the graphene oxide at80-150 DEG C by using sodium borohydride as a reducer by the aid of a catalyst, oxygen-containing functional groups (epoxy group, hydroxy group, carboxy group and carbonyl group) on the graphene oxide are removed, and the electric conductivity of the graphene is thoroughly recovered, thereby preparing the graphene. The process disclosed by the invention is suitable for large-scale industrial production. The process has the advantages of low reduction temperature, mild and controllable reaction, thorough reduction, environment friendliness and the like, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of graphene, and in particular relates to a method for preparing graphene by a low-temperature chemical method, specifically a method for preparing a graphite nanomaterial with a single carbon atom thickness by low-temperature catalytic reduction. The graphene prepared by this method can be widely used in the fields of microelectronic devices, sensors and new energy materials. Background technique [0002] Graphene is a flake graphite material with a thickness of one carbon atom discovered by British scientists in 2004. Due to the long-range π-conjugated bonds of graphene, it has excellent properties in electricity, mechanics, and heat. It will be a new material with a wide range of uses, and it is a current research hotspot. [0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, chemical vapor deposition method, epitaxial growth method, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
CPCC01B32/198B01J21/04B01J27/10C01B32/184C01B2204/22
Inventor 林红李俊峰李建保
Owner TSINGHUA UNIV
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