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Method for preparing high-quality large-size graphene on large scale

A large-scale preparation and graphene technology, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve the problems of low production efficiency and long ball milling time, and achieve the goal of improving production efficiency, short ball milling time, and avoiding impurities Effect

Active Publication Date: 2019-12-10
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this patent, graphite is ball-milled in order to reduce the thickness of graphite. The ball-milling time is long, ranging from 1 to 20 hours, and the production efficiency is low. At the same time, the graphene precursor is mixed with a solvent before wet ball-milling. The solvent includes deionized water, Any one or a combination of at least two of N-methylpyrrolidone, N,N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone or 4-butyrolactone

Method used

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  • Method for preparing high-quality large-size graphene on large scale
  • Method for preparing high-quality large-size graphene on large scale
  • Method for preparing high-quality large-size graphene on large scale

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Take by weighing 1g 80 mesh original graphite powder and put it into the ball mill jar of planetary ball mill, and add an appropriate amount of mass fraction therein to be 10% perchloric acid solution, the addition is to reach two-thirds of the ball mill jar as the criterion, and then add Fill the ball mill jar with argon and seal it, put it into a planetary ball mill and react for 1 hour with 200 rpm ball mill, filter and collect the perchloric acid solution with a mass fraction of 10% for reuse, and grind the graphite powder after ball milling at 80 After fully drying in a blast drying oven at ℃, take 2 ml of perchloric acid solution with a mass fraction of 72% and mix it evenly in a crucible, then place the crucible in a tube furnace and heat it to 170 °C under an argon protective atmosphere Insulate for 1h, after the tube furnace cools down, ultrasonically disperse the obtained graphene aggregates in absolute ethanol with a purity of 99%, and finally dry in air to ob...

Embodiment 2

[0041]Take by weighing 1g 32 order original graphite powders and put into the ball mill jar of planetary ball mill, and add the perchloric acid solution that an amount of mass fraction is 10% wherein, the addition is to reach two-thirds place of ball mill jar as the criterion, then Fill the ball mill jar with argon and seal it, put it into a planetary ball mill and react for 2 hours at 100 rpm, filter and collect the perchloric acid solution with a mass fraction of 10% for reuse, and grind the graphite powder at 80 After fully drying in a blast drying oven at ℃, take 2 ml of perchloric acid solution with a mass fraction of 72% and mix it evenly in a crucible, then place the crucible in a tube furnace and heat it to 200 °C under an argon protective atmosphere Keep warm for 1h, after the tube furnace cools down, ultrasonically disperse the obtained graphene aggregates in absolute ethanol with a purity of 99%, and finally dry in air to obtain a size of 160 μm 2 , with a conductiv...

Embodiment 3

[0043] Take by weighing 0.05g 500 mesh original graphite powder and put it into the ball milling jar of planetary ball mill, and add an appropriate amount of mass fraction therein to be 10% perchloric acid solution, the addition is to reach two-thirds of the ball milling jar as the criterion, then Fill the ball mill jar with argon and seal it, put it into a planetary ball mill and react for 0.5h with 500 rpm ball mill, filter and collect the perchloric acid solution with a mass fraction of 10% for reuse, and put the ball milled graphite powder in After being fully dried in a blast drying oven at 80°C, measure 1 ml of perchloric acid solution with a mass fraction of 72% and mix it evenly in a crucible, then place the crucible in a tube furnace and heat it to 180 °C under an argon protective atmosphere. ℃ for 0.5h, after the tube furnace is cooled, the obtained graphene aggregates are ultrasonically dispersed in absolute ethanol with a purity of 99%, and finally dried in the air ...

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Abstract

The invention discloses a method for preparing high-quality large-size graphene on a large scale, and belongs to the technical field of novel materials. The method comprises the steps of carrying outball-milling on original graphite powder for a short time to damage edge structures of graphite; and then carrying out oxidative intercalation stripping at the low temperature to obtain the graphene.The method is simple and practicable, and the yield nearly reaches 100%; and meanwhile, a solvent during ball-milling and a subsequent intercalation agent are perchloric acid solutions, so that the solvent and the subsequent intercalation agent can be reused, and the cost is saved; and water washing and waste liquid discharging processes are not involved, and waste of water resources and pollutionof waste liquid to the environment are avoided.

Description

technical field [0001] The invention relates to a method for preparing graphene, which belongs to the technical field of new materials. Background technique [0002] Graphene, a carbon nanomaterial with a honeycomb two-dimensional lattice structure, has attracted widespread attention since it was discovered by Andre Geim and Konstantin Novoselov in 2004. Its unique two-dimensional structure enables it to exhibit unusual properties in terms of electrical conductivity, thermal conductivity, and mechanics, thus demonstrating its broad application prospects in batteries, sensors, flexible electronics, and functional composite materials. [0003] However, how to achieve large-scale preparation of high-quality graphene is still an important bottleneck restricting its application. The existing preparation methods mainly include chemical vapor deposition, redox, electrochemical and liquid phase exfoliation. Among them, the chemical vapor deposition method is usually expensive and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/32C01B2204/22
Inventor 张瑞军吴文玉
Owner YANSHAN UNIV
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