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Method for preparing single-layer graphene through mechanical method

A single-layer graphene, mechanical method technology, applied in the direction of single-layer graphene, graphene, chemical instruments and methods, etc., can solve the problems of high iron impurity content in products, long ball milling time, low success rate, etc. Short, high success rate, high yield effect

Inactive Publication Date: 2017-08-25
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, In-Yup Jeon et al. (In-Yup Jeon, Yeon-Ran Shin et al.PNAS: Edge-carboxylated graphene nanosheets via ball milling, 2012,109:5588-5593) prepared single-layer graphene by ball milling , activate dry ice and natural flake graphite in a ball mill for 48 hours to obtain edge carboxylated graphene flakes, but this method has low success rate, long ball milling time, high energy consumption, high content of iron impurities in the product, and the product has no decarboxylation

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  • Method for preparing single-layer graphene through mechanical method
  • Method for preparing single-layer graphene through mechanical method
  • Method for preparing single-layer graphene through mechanical method

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Embodiment 1

[0024] The specific steps of the method for preparing single-layer graphene by mechanical method involved in the present embodiment are:

[0025] (1) Carboxylation: Place the natural flake graphite powder in a vacuum drying oven at a temperature controlled at 50°C for 24 hours in a vacuum, take it out after cooling to room temperature, and accurately weigh 5g of the cooled natural flake graphite powder, 105g of dry ice, and 300g in diameter. 5mm stainless steel balls and 250g stainless steel balls with a diameter of 7.5mm are placed together in a sealed ball mill jar and quickly seal the ball mill jar; after the air pressure of the pressure gauge in the ball mill jar is stabilized, adjust the deflation valve to slowly deflate to control the gas Flow 10—20cm 3 / min, 450r / min ball milling for 24h, after the air pressure in the pressure gauge drops to 0, continue ball milling for 6h, open the ball milling tank to expose the natural flake graphite powder to the air to absorb moist...

Embodiment 2

[0030] The specific steps of the method for preparing single-layer graphene by mechanical method involved in the present embodiment are:

[0031] (1) Carboxylation: Place the natural flake graphite powder in a vacuum drying oven at a temperature controlled at 50°C for 24 hours in vacuum, take it out after cooling to room temperature, and accurately weigh 5g of the dried natural flake graphite powder, 105g of dry ice, and 300g in diameter. 5mm stainless steel balls and 250g stainless steel balls with a diameter of 7.5mm are placed together in a sealed ball mill jar and quickly seal the ball mill jar; after the air pressure of the pressure gauge 1 in the ball mill jar is stabilized, adjust the air release valve 2 to deflate slowly, Control gas flow 10-20cm 3 / min, 450r / min ball milling 24h, continue ball milling 6h after the air pressure drops to 0 in pressure gauge 1, open the sealing cover 4 of ball mill jar and make natural flake graphite powder expose in the air to absorb mo...

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Abstract

The invention belongs to the technical field of graphene preparation and relates to a method for preparing single-layer graphene through a mechanical method. A specific technological process of the method comprises three steps of a hydroxylation process, a decontaminating process and a reduction process. The edge of natural flake graphite is processed in a carboxylation mode through a ball milling method to obtain initial carboxylation graphene powder, then pure carboxylation graphene powder with small iron content is obtained through the decontaminating process, and high-quality single-layer graphene is obtained through the thermal reduction process. The method avoids any strong oxidant and has high carboxylation degree, short ball milling time and high success rate; the decontaminating process is simple and effective; the reduction process avoids using reducing agents and is environmentally friendly; a main structure of a ball milling tank related to the hydroxylation process comprises a pressure meter, a gas exhaust valve, a tank body, a sealing cover and a stainless steel ball. The method has high preparation success rate, large yield, no pollution and low energy consumption and can achieve large-scale mechanical production through amplifying ball milling equipment.

Description

[0001] Technical field: [0002] The invention belongs to the technical field of graphene preparation, and relates to a method for preparing high-quality single-layer graphene by a mechanical method, which can better realize large-scale application. [0003] Background technique: [0004] Graphene is the material with the highest strength, the best toughness, the lightest weight, the highest light transmittance, and the best conductivity known to mankind. It is used in heat dissipation materials, energy storage materials, electronic devices, conductive inks, anti-corrosion coatings, flexible Display screens, composite materials and other fields have broad application prospects. The large-scale production of graphene has always been a key factor restricting the industrial development and large-scale application of graphene. At present, the preparation of single-layer graphene roughly includes the following methods: first, oxidation-reduction method; second, chemical vapor deposi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/19
CPCC01B2204/02C01B2204/04C01B2204/32C01P2004/04
Inventor 于希萌
Owner QINGDAO UNIV
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