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Method for preparing graphene by reduction of sulfur-contained compound

A technology of graphene and compounds, which is applied in the field of graphene products prepared by chemical reduction method, can solve the problems of difficulty in obtaining high-quality graphene, low conductivity of graphene, and low conductivity of graphene, and achieve a green and efficient preparation method. The preparation is safe and simple, and the effect of high C/O ratio

Inactive Publication Date: 2013-01-30
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The preparation methods of graphene reported above all have defects in varying degrees, such as hydrazine, hydrazine hydrate, or sodium borohydride have high toxicity and danger, and are also prone to high nitrogen doping in the graphene produced, affecting Graphene purity
However, when amino acids or vitamins are used as reducing agents, the conductivity of graphene obtained is low, and it is difficult to obtain high-quality graphene. The graphene prepared by thermal and microwave reduction also has the problem of low conductivity.

Method used

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  • Method for preparing graphene by reduction of sulfur-contained compound
  • Method for preparing graphene by reduction of sulfur-contained compound
  • Method for preparing graphene by reduction of sulfur-contained compound

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 50 mg of graphene oxide to 50 ml of deionized water, and ultrasonicate it in an ultrasonic bath for 5 minutes to make it uniformly disperse into a yellow liquid, then add 1.35 or 2.7 mmol of reducing agent NaHSO 3 After uniform dispersion, the temperature was raised to 95°C, and the reaction was maintained for 3 hours under stirring. After the reaction was completed, it was lowered to room temperature and filtered with suction to obtain a black filter cake, which was washed 4 times with 50 ml of water, and then freeze-dried to obtain graphene powder.

[0028] figure 1 The photos of graphene oxide (a) and reduced graphene (b) are given. It can be seen that the obtained graphene is a black powder. Elemental analysis shows that the C / O ratio of graphene obtained is 7.89, and the degree of reduction is high. . It can also be seen that the method can realize batch preparation of graphene.

[0029] figure 2 It is the C1s collection of graphene (CRG) obtained in the p...

Embodiment 2

[0036] In this example, 50 mg of graphene oxide was added to 50 ml of deionized water, and ultrasonicated in an ultrasonic bath for 5 minutes to uniformly disperse it into a yellow liquid, and then 5.0 mmol of reducing agent Na 2 S·9H 2 O, after uniform dispersion, the temperature was raised to 95°C, and the reaction was maintained for 3 hours under stirring. After the reaction was completed, it was lowered to room temperature and filtered with suction to obtain a black filter cake, which was washed 4 times with 50 ml of water, and then freeze-dried to obtain graphene powder.

Embodiment 3

[0038] In this example, 50 mg of graphene oxide was added to 50 ml of deionized water, and ultrasonicated in an ultrasonic bath for 5 minutes to uniformly disperse it into a yellow liquid, and then 5.0 mmol of reducing agent Na 2 S 2 o 3 After uniform dispersion, the temperature was raised to 95°C, and the reaction was maintained for 3 hours under stirring. After the reaction was completed, it was lowered to room temperature and filtered with suction to obtain a black filter cake, which was washed 4 times with 50 ml of water, and then freeze-dried to obtain graphene powder.

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Abstract

The invention discloses a method for preparing graphene by reduction of a sulfur-contained compound, which concretely comprises the following steps of: dispersing graphene oxide into deionized water or a mixed solution of the deionized water and N,N-dimethylacetylamide to obtain uniform dispersing liquid with the concentration of 1-3mg / ml; then adding 1.35-5mmol of sulfur-contained compound and making the mixture react at 94-96 DEG C for 1-3 hours; and enabling the reaction product to be subjected to the processes of filtration, washing, frozen drying, and the like to obtain high-purity grapheme. The invention has the advantages of simple and safe process and high quality of the grapheme prepared by adopting the method and can be widely used for the preparation of novel grapheme, materials and devices.

Description

technical field [0001] The invention belongs to the technical field of preparing graphene products by a chemical reduction method, and in particular relates to a method for preparing graphene by reducing a sulfur-containing compound. Background technique [0002] Graphene is a two-dimensional graphite material with a single molecular layer. It has attracted much attention because of its potential high electrical conductivity, thermal stability, mechanical strength and special quantum properties. It is considered to be a new material that will fully replace silicon in the future. As the basis of application, the current preparation technology of graphene still has a lot of room for development. The current graphene preparation methods mainly include mechanical exfoliation, chemical vapor deposition (CVD), and chemical reduction. Among them, the chemical reduction method has been paid more attention because of its simple process and easy batch preparation. The basic process ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B82B3/00C01B31/04
Inventor 闫立峰陈武峰
Owner UNIV OF SCI & TECH OF CHINA
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