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Method for electrochemically preparing low-oxygen-content graphene

A technology with low oxygen content and graphene, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve the problems of large amounts of waste water or waste gas, low graphene output, low production efficiency, etc., and achieve easy industrialization, Effect of protecting graphene and mild conditions

Pending Publication Date: 2020-05-29
GUILIN UNIV OF ELECTRONIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among these methods, the preparation efficiency of mechanical exfoliation method and crystal epitaxial growth method is relatively low, and it is currently difficult to meet the needs of large-scale production; chemical vapor deposition method is only suitable for electronic devices and transparent conductive films, but it cannot meet the needs of energy storage materials and functions. Large-scale demand in the field of composite materials; graphene prepared by the oxidation-reduction method usually contains more defects, and a large amount of waste water or waste gas will be generated during the preparation process, causing serious pollution to the environment; the output of graphene prepared by microwave method It is not yet possible to achieve large-scale industrial production

Method used

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  • Method for electrochemically preparing low-oxygen-content graphene
  • Method for electrochemically preparing low-oxygen-content graphene
  • Method for electrochemically preparing low-oxygen-content graphene

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Embodiment 1

[0028] First, dissolve the electrolyte sodium benzenesulfonate in 100ml deionized water, then mix it with 100ml hydrogen peroxide and stir evenly to prepare an electrolyte solution; finally, the concentration of the electrolyte sodium benzenesulfonate in the electrolyte solution is 0.1mol / L, and then the graphite foil Insert the platinum electrode into the electrolyte solution, apply a voltage of 30V with a power supply, electrolyze for 30min, wash with deionized water and absolute ethanol several times in sequence to obtain the initial graphene product, and dry it in vacuum; then add water for 30min and ultrasonic power is 40W, and finally Stand still for 12 hours, remove the precipitate, take the supernatant, and finally obtain graphene with an oxygen content of 6.3%, a thickness of 2.4-3nm, and a lateral size of 3-8um.

Embodiment 2

[0030] First, the electrolyte naphthalene-1,5-sodium disulfonate was dissolved in 100ml of deionized water, then mixed with 100ml of hydrogen peroxide and stirred evenly to prepare an electrolyte solution; finally the concentration of the electrolyte sodium benzenesulfonate in the electrolyte solution was 0.2mol / L, then insert the graphite foil and the platinum electrode into the electrolyte solution, apply a voltage of 20V with the power supply, electrolyze for 30min, wash several times with deionized water and absolute ethanol successively, obtain the initial product of graphene, vacuum dry; then add water and ultrasonic for 30min, The ultrasonic power was 40W, and finally stood still for 12 hours, the precipitate was removed, and the supernatant was taken to finally obtain graphene with an oxygen content of 4%. The thickness is 1.7-2.8nm, and the lateral dimension is 3-5um.

Embodiment 3

[0032] First, dissolve the electrolyte ammonium sulfate in 100ml of deionized water, then mix it with 100ml of hydrogen peroxide and stir evenly to prepare an electrolyte solution; finally, the concentration of the electrolyte sodium benzenesulfonate in the electrolyte solution is 0.3mol / L, and then the graphite foil and platinum Insert the electrode into the electrolyte solution, apply a voltage of 30V with the power supply, electrolyze for 30min, wash with deionized water and absolute ethanol several times in sequence, and obtain the primary graphene product, and dry it in vacuum; then add water and ultrasonically for 30min, the ultrasonic power is 40W, and finally let it stand After 12 hours, the precipitate was removed, and the supernatant was taken to finally obtain graphene with an oxygen content of 7.5%, a thickness of 1.5-2.4nm, and a lateral size of 2-5um.

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Abstract

The invention discloses a method for electrochemically preparing low-oxygen-content graphene. Non-toxic organic salt is used as an electrolyte to carry out electrochemical stripping on a graphite foil. As a stripping aid and a protective agent, hydrogen peroxide can generate gas to help stripping of graphene in the stripping process, meanwhile, the hydrogen peroxide is used as a reducing agent toreact with free radicals in a system to reduce the reaction between the free radicals and the graphene, so that the purpose of protecting the graphene is achieved, and finally, a low-oxygen-content graphene product with relatively high quality, the thickness of 1.3-3.2nm and the maximum transverse size of 8 microns can be obtained. The method has the advantages of mild process conditions, no toxicreagents in the whole process, no pollution to the environment, simple operation and easy industrialization, the introduction of the electrolyte and hydrogen peroxide can ensure that the structure and performance of graphene are not destroyed, and the prepared graphene is low in oxygen content.

Description

Technical field: [0001] The invention relates to the technical field of carbon materials, in particular to a method for electrochemically preparing graphene with low oxygen content. Background technique: [0002] Graphene is made of sp 2 A honeycomb two-dimensional atomic crystal composed of hybridized carbon atoms. Each carbon atom is connected to the other three atoms through a σ bond, and the remaining P orbital electrons form a π bond. The six-membered ring formed by conjugated carbon atoms can be regarded as its structural unit. Graphene can be regarded as an atomic-scale network composed of carbon atoms and their covalent bonds, and the huge conjugated structure is also considered as a polycyclic aromatic hydrocarbon. Because graphene has many advantages such as ultra-high carrier mobility, electrical conductivity, thermal conductivity, light transmittance, and mechanical strength, it is widely used in lithium-ion batteries, supercapacitors, solar cells, seawater des...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19C01B2204/32C01B2204/04
Inventor 张坚刘建张哲泠
Owner GUILIN UNIV OF ELECTRONIC TECH
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