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Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt

A technology for exfoliating graphite and graphene, which is applied in the field of preparing graphene by electrochemically exfoliating graphite materials with molten salt, can solve the problems of long time for electrochemical exfoliation, low yield, high cost, etc., and achieve the convenience of large-scale production and equipment requirements Simple, wide-ranging effects of graphite raw materials

Inactive Publication Date: 2015-01-21
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Micromechanical exfoliation can produce high-quality graphene, but it has the disadvantages of low yield and high cost, which does not meet the requirements of industrialization and large-scale production
The preparation cost of redox method is low and easy to realize, and stable graphene suspension can be prepared, which solves the problem that graphene is not easy to disperse, and the method of gas-liquid self-assembly can produce good quality graphene sheet material (Self -Assembled Free-Standing Graphite Oxide Membrane.Adv.Mater.(2009), 21,3007-3011), but redox graphene has heteromembered rings and non-carbon-based functional groups, which limits the application of redox graphene
Invention patent "A method for preparing graphene from electrochemically swollen graphite" (application number: CN201310659172.5) adopts the method of combining solvent stripping and electrochemistry, using sodium perchlorate, aluminum nitrate, water and dimethyl carbonate as Electrolyte can be used to prepare graphene in large quantities. The disadvantage of this method is that the electrochemical stripping takes a long time, and the time taken in the examples reaches 48-72h

Method used

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  • Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt
  • Method for preparing graphene by peeling graphite in electrochemical manner by using molten salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) Mix sodium chloride, potassium chloride and aluminum chloride in a ratio of 1:1:8, heat the mixed salt to 150°C, and keep the temperature constant so that the mixed salt is completely melted;

[0023] 2) Fix the flake graphite to the positive pole of the power supply and the aluminum plate to the negative pole of the power supply by using a polytetrafluoroethylene net, and place them in the molten salt obtained in 1);

[0024] 3) Use a DC stabilized power supply to pass a constant current to the electrodes in 2), with a current density of 3A dm -2 . When the reaction time is 2h, turn off the power;

[0025] 4) When the temperature drops to room temperature, wash the reaction product of 3) with water, so that the pH of the product cleaning solution is neutral, let it stand for 1 hour, and take the suspension;

[0026] 5) Ultrasonic shock treatment was performed on the suspension in 4) for 60 minutes, and left to stand for 72 hours to obtain a secondary suspension; ...

Embodiment 2

[0029] 1) Mix sodium chloride, potassium chloride and aluminum chloride at a ratio of 20:14:66, heat the mixed salt to 150°C, and keep the temperature constant so that the mixed salt is completely melted;

[0030] 2) Fix the flake graphite to the positive pole of the power supply and the aluminum plate to the negative pole of the power supply by using a polytetrafluoroethylene net, and place them in the molten salt obtained in 1);

[0031] 3) Use a DC stabilized power supply to pass a constant current to the electrode in 2), and the current density is 2A·dm -2 . When the reaction time is 2h, turn off the power;

[0032] 4) When the temperature drops to room temperature, wash the reaction product of 3) with water, so that the pH of the product aqueous solution is neutral, let it stand for 1 hour, and take the suspension;

[0033] 5) The suspension in 4) was subjected to ultrasonic shock treatment for 60 minutes, and left to stand for 24 hours to obtain a secondary suspension;...

Embodiment 3

[0036] 1) Mix sodium chloride, potassium chloride and aluminum chloride at a ratio of 20:14:66, heat the mixed salt to 150°C, and keep the temperature constant so that the mixed salt is completely melted;

[0037] 2) using flexible graphite as an anode and an aluminum plate as a cathode, placing them in the molten salt obtained in 1);

[0038] 3) Use a DC stabilized power supply to pass a constant current to the electrodes in 2), with a current density of 3A dm -2 . When the reaction time is 2h, turn off the power;

[0039] 4) When the temperature drops to room temperature, wash the reaction product of 3) with water, so that the pH of the product aqueous solution is neutral, let it stand for 1 hour, and take the suspension;

[0040] 5) The suspension in 4) was subjected to ultrasonic shock treatment for 60 minutes, and left to stand for 24 hours to obtain a secondary suspension;

[0041] 6) The suspension in 5) was vacuum-dried at 100° C. for 10 h to obtain graphene.

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Abstract

The invention discloses a method for preparing graphene by peeling graphite in an electrochemical manner by using molten salt. The method is characterized by combining an electrochemical method and a solvent method. According to the method, molten salt is used as a peeling medium, and the peeling power is provided by migration of charge particles in the molten salt. According to the technical scheme, the method comprises the following three steps: (1) preparing mixing salt of aluminum chloride, sodium chloride and potassium chloride of appreciate ratio, heating to be 150 DEG C, and keeping the temperature; (2) respectively introducing appreciate current into graphite and an aluminum electrode for electrochemical peeling; and (3) separating the graphene which is obtained by peeling by using the molten salt. The method has the advantages that the graphene defects are small, the equipment requirements are small, the graphene can be rapidly and massively prepared, the industrialization is easy to achieve, and the like.

Description

technical field [0001] The patent of the present invention relates to a method for preparing graphene, in particular to a method for preparing graphene by electrochemically exfoliating graphite materials with molten salt. Background technique [0002] Graphene is composed of a single layer of carbon atoms with sp 2 The nanomaterial with a hexagonal lattice honeycomb structure formed by hybridization bonding belongs to a new type of two-dimensional crystal material. Graphene has good electrical conductivity, thermal conductivity, optical transparency, and special mechanical and electronic properties. It has good application prospects in energy storage, transparent conductive devices, composite materials, and optoelectronic devices. Therefore, graphene has become a research hotspot in the fields of materials science, physics and chemistry. In terms of industrialization, the development of graphene products has also made remarkable progress in recent years due to the developm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 马兆昆曹瑞雄宋怀河
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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