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Method for preparing graphene

A technology of graphene and graphite micropowder, which is applied in the direction of graphene and nano-carbon, which can solve the problems of harsh preparation conditions, long time-consuming, and incomplete repair, and achieve the effect of less graphene defects, no waste water, and high peeling efficiency

Inactive Publication Date: 2012-07-11
DALIAN LICHANG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The first three methods are difficult to apply to large-scale production of graphene due to low yield and harsh preparation conditions
The chemical redox method is currently considered to have the most potential to achieve large-scale preparation. However, because the oxidation process in this method destroys the structure of graphene, and the reduction process cannot completely repair its structure, resulting in various graphene preparations. The excellent performance cannot be fully reflected, and at the same time, there is a problem of wastewater generation during the oxidation process
Although the reported intercalation exfoliation method does not destroy the graphene layer structure in the graphite raw material, it generally has disadvantages such as low yield and long time consumption. How to effectively improve the efficiency of the intercalation exfoliation method is a problem that needs to be solved

Method used

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Embodiment 1

[0020] Embodiment 1: 0.5 gram of natural flake graphite (purity>99%, D50=18 microns) is added to 10 milliliters of N, in the mixed solvent of N-dimethylformamide (DMF) and propylene carbonate (PC) (3 : 1 volume ratio), then add 0.5 gram of sodium hydroxide, carry out ultrasonic treatment with VCX-750 (Sonic & Materials Inc) ultrasonic equipment for 35 hours (ultrasonic frequency 20KHz), control the temperature range at 20-100 ° C, filter, and then successively Wash with deionized water, DMF, and vacuum dry to obtain a mixed product (1≤n≤5) composed of n atomic layer graphene.

Embodiment 2

[0021] Embodiment 2: 0.2 gram of natural flake graphite (purity>99%, D50=50 microns) is added in the mixed solvent of 10 milliliters of N-methylpyrrolidone (NMP) and propylene carbonate (PC) (2: 1 volume ratio ), then add 0.2 grams of KCl, and use VCX-750 ultrasonic equipment to perform ultrasonic treatment for 20 hours (ultrasonic frequency 10KHz), control the temperature range at 20-100 ° C, centrifuge, then successively wash with deionized water, NMP, and vacuum dry to obtain Hybrid products (1≤n≤5) consisting of n atomic layers of graphene.

Embodiment 3

[0022] Embodiment 3: 1 gram of natural flake graphite (purity > 99%, D50=100 microns) is added to 10 milliliters of N, in the N-dimethylformamide (DMF) solvent, then add 0.5 gram of LiPF 6 , use VCX-750 ultrasonic equipment to carry out ultrasonic treatment for 50 hours (ultrasonic frequency 20KHz), control the temperature range at 20-100 ° C, filter, then wash with deionized water, DMF, and vacuum dry to obtain graphene composed of n atomic layers Mixed products (1≤n≤5).

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Abstract

The invention relates to a method for preparing graphene, belonging to the field of the preparation of inorganic non-metallic material powder. The method comprises the following steps of: taking natural flake graphite powder with a certain grain size as a raw material; adding the natural flake graphite powder into an organic solvent dissolved with alkali metal compounds, and carrying out ultrasonic dispersion processing (the ultrasonic frequency is no less than 10 KHz); filtering or carrying out centrifugal separation; washing; and carrying out vacuum drying to obtain a mixed product formed by the graphene with n atomic layers, wherein n is no less than 1 and no more than 5. In order to increase the peeling ratio, the natural flake graphite powder with the certain grain size can be prepared into a lithium battery cathode material by serving as a raw material, after the lithium battery cathode material is charged by a lithium battery to activate, the lithium battery cathode material is peeled from a current collector and is collected, and then, the ultrasonic dispersion processing is carried out. Compared with the prior art, the method for preparing the graphene has the advantages of simple operating process, easiness in enlarged production, high peeling efficiency, little graphene defects and no generation of wastewater.

Description

technical field [0001] The invention relates to a preparation method of graphene, which belongs to the field of preparation of inorganic non-metallic material powder. Specifically, the present invention relates to a method for preparing a mixed product (1≤n≤5) composed of n atomic layer graphene by using natural graphite as a raw material and undergoing one-step ultrasonic treatment. Background technique [0002] Since it was discovered by British scientists in 2004, graphene has become one of the hot spots in the field of material research in recent years due to its unique structure, excellent performance, high theoretical research value, and broad application prospects. Graphene has a two-dimensional honeycomb crystal structure composed of a single layer of carbon atoms closely packed, which makes it have excellent electrical, mechanical, thermal and optical properties. For example, graphene has an ultra-high carrier mobility 100 times that of silicon. Rate, up to 130GPa ...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/19
Inventor 耿世达陈杨英楚合磊孙振伟杨金凤
Owner DALIAN LICHANG NEW MATERIAL CO LTD
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