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Electrochemical preparation method of graphene

An electrochemical and graphene technology, applied in the electrolysis process, electrolysis components, etc., can solve the problems of complicated and lengthy process, expensive equipment, and many graphene defects, and achieve high quality, high stripping efficiency and yield, and few defects. Effect

Inactive Publication Date: 2013-12-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a low-cost, high-quality, simple and easy-to-operate graphene material preparation method for the graphene prepared by the prior art with many defects, complicated and lengthy process or expensive equipment.

Method used

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  • Electrochemical preparation method of graphene

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example 1

[0019] 20 mg of graphite powder was pressed into a graphite sheet (8 mm X 6 mm) by direct compression method, and then wrapped in a stainless steel mesh. Such as figure 1 In the diagram of the experimental device shown, the anode and cathode are self-made graphite sheet electrodes, the electrolyte is 1-methylimidazolium bisulfate, and a voltage of 4V is continuously applied for 5 hours. Transfer the cathode and anode expanded graphite into two agate mortars respectively, add 0.2ml of 1-methylimidazolium bisulfate, and grind for 3 hours. The gel-like mixture was transferred into a mixed solvent of acetone and DMF (V:V=2:1), and washed by high-speed centrifugation for 3 times to remove, the rotation speed was 13000rmp, and each time was 10min. The sediment was transferred into 50ml DMF, centrifuged at 2000rmp for 5min, and the supernatant was the obtained graphene solution, which was dark gray.

[0020] Such as figure 1 Raman diagram, Figure a is the graphene produced by the ...

example 2

[0022] Such as figure 1 In the diagram of the experimental device shown, both the anode and cathode are 20mg highly pyrolytic graphite sheets, the electrolyte is 1-butyl-3-methylimidazolium bisulfate, and a voltage of 5v is continuously applied for 5 hours. Transfer the cathode and anode expanded graphite into two agate mortars respectively, add 0.3ml of 1-butyl-3-methylimidazolium bisulfate, and grind for 3 hours. The gel-like mixture was transferred into a mixed solvent of acetone and DMF (V:V=1.5:1), and washed by high-speed centrifugation for 3 times to remove, the rotation speed was 13000rmp, and each time was 10min. The sediment was transferred into 50ml DMF, centrifuged at 5000rmp for 5min, and the supernatant was the prepared graphene solution, which was gray.

example 3

[0024] 20 mg of graphite powder was pressed into a graphite sheet (8 mm X 6 mm) by direct compression method, and then wrapped in a stainless steel mesh. Such as figure 1 In the diagram of the experimental device shown, the cathode and anode are self-made graphite sheet electrodes, the electrolyte is 1-butyl-3-methylimidazolium dihydrogen phosphate, and a voltage of 6V is continuously applied for 4.5 hours. Transfer the cathode and anode expanded graphite into two agate mortars respectively, add 0.5ml of the above-mentioned 1-butyl-3-methylimidazolium dihydrogen phosphate, and grind for 6 hours. The gel-like mixture was transferred into a mixed solvent of acetone and DMF (V:V=2.5:1), and washed by high-speed centrifugation for 3 times to remove, the rotation speed was 13000rmp, and each time was 10min. The sediment was transferred into 50ml DMF, centrifuged at 2000rmp for 5min, and the supernatant was the prepared graphene solution, which was gray.

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Abstract

The invention provides an electrochemical preparation method of a graphene material. The preparation method comprises the following steps: using graphite electrodes as negative and positive electrodes respectively and one or more of 1-butyl-3-methylimidazolium dihydrogenphosphate, N-methyl pyrrolidone hydrosulfate, N-methyl pyrrolidone dihydrogenphosphate and 1-methylimidazolium hydrosulfate as an electrolyte, applying voltage of 3.1-6.0V, and obtaining highly expanded graphite at the negative and positive electrodes respectively; then adding the corresponding electrolyte to the expanded graphite according to (100:1)-(30:1), grinding for 3-6 hours, then transferring the expanded graphite to acetone and dimethyl formamide mixed liquor, carrying out centrifugation at 13000rpm, transferring the precipitate to dimethyl formamide, and carrying out centrifugation at 2000-10000rpm, thus obtaining a supernatant, namely a stable graphene solution, wherein the volume ratio of acetone to dimethyl formamide is (1.1:1)-(3:1). The preparation method has the beneficial effects that the preparation process of the graphene material produced by the preparation method is mild and simple and has a defect cure phenomenon, and the product graphene has few defects and high quality.

Description

technical field [0001] The invention relates to a method for preparing graphene materials related to the technical field of nanometer materials, in particular to a method for obtaining graphene materials in a new processing manner. Background technique [0002] Graphene is a two-dimensional atomic crystal material composed of a single layer of closely arranged carbon atoms. In 2004, the graphite monolithic sheet was obtained by the scientist Geim A K et al. by repeatedly peeling off the graphite sheet through tape. Before the discovery of graphene, it was believed theoretically and experimentally that the perfect two-dimensional structure could not exist stably at non-absolute zero temperature, so the discovery of graphene attracted the attention of the whole world, and its discoverer won the Nobel Prize in 2010 Physics Prize. [0003] In fact, graphene is the building block of carbon-based materials in other dimensions. Zero-dimensional fullerenes can be regarde...

Claims

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Application Information

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IPC IPC(8): C25B1/00
Inventor 刘洪涛毛敏
Owner CENT SOUTH UNIV
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