Preparation method of high quality graphene conductive film

A technology of graphene and conductive film, applied in the field of preparation of high-quality graphene conductive film, can solve problems such as complex process, low conductivity, pollution, etc., achieve high controllability of process parameters, simple preparation method, and wide application prospects Effect

Active Publication Date: 2015-04-29
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation methods of graphene mainly include mechanical exfoliation method, chemical vapor deposition method, epitaxial growth method, solvent exfoliation method and chemical redox method. It is not suitable for large-scale industrial production of graphene; chemical vapor deposition and epitaxial growth methods have disadvantages such as complex process, harsh conditions, low yield, and high cost, which limit their large-scale industrial production and application of graphene; epitaxial growth The method is used to grow graphene by heating SiC epitaxy for electronic devices, etc., but because the SiC crystal surface is prone to reconstruction during the heating process, it is difficult to obtain large-area uniform graphene, and the heating temperature is high and energy consumption is large; the solvent stripping method The stripping efficiency and yield are low, and there are few applicable solvents; the chemical redox method is currently a low-cost, large-scale method for preparing graphene, but the strong oxidizing agent used in the stripping process of the chemical stripping method will destroy the graphene carbon. The planar structure of atoms produces defects, which lead to a decrease in the conductivity of graphene, and toxic chemicals such as hydrazine hydrate, which are usually used in the reduction process, are likely to pollute the environment
However, the graphene film prepared by redox method has low electrical conductivity, many defects, and poor mechanical properties; and the solvent dispersibility and film-forming property of graphite bulk material are poor; Good stability and film-forming properties, but poor conductivity and high resistance

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  • Preparation method of high quality graphene conductive film
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  • Preparation method of high quality graphene conductive film

Examples

Experimental program
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Embodiment 1

[0023] The concrete steps that present embodiment prepares high-quality graphene conductive film are:

[0024] (1), 10g of natural graphite with a sheet diameter of 100 μm is added to a mixed acid composed of 10ml of concentrated nitric acid (65%) and 30ml of concentrated sulfuric acid (98%) and mixed evenly, then 20g of ferric chloride is added, and the reaction is stirred and reacted at 35 degrees for 12h , filtered, washed with water to pH=7, and dried at 60 degrees Celsius for 8 hours to obtain layered graphite;

[0025] (2), process the layered graphite under 1000w microwave for 3min to obtain the graphite after microwave treatment, the graphite will expand during the treatment process, accompanied by sparks;

[0026] (3), the graphite after the microwave treatment is dispersed in water, and ultrasonically peeled off for 60min at 500w to obtain a graphene aqueous solution with a concentration of 0.5-2mg / ml;

[0027] (4), centrifuge 100ml of graphene aqueous solution with...

Embodiment 2

[0034] The other steps of this embodiment are the same as in Example 1, only when the intercalation agent is added, the intercalation agent added is ammonium nitrate, potassium chlorate, lithium chlorate, potassium oxalate, ammonium oxalate, ammonium carbonate, ammonium bicarbonate, sodium carbonate, One or more of sodium bicarbonate, potassium bicarbonate and iron carbonate, the amount added is the same as ferric chloride, and the performance of the graphene conductive film obtained at last is similar to that of the graphene conductive film obtained in Example 1.

Embodiment 3

[0036] The other steps of this embodiment are the same as in Example 1, only in the film-forming process, the concentration of the ethanol dispersion of graphene is 20 mg / ml, the thickness of the obtained graphene conductive film is 20 μm, and the conductivity is 20000 S / m.

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Abstract

The invention belongs to the technical field of graphene materials and relates to a preparation method of a high quality graphene conductive film. The preparation method comprises the following steps: uniformly mixing natural flake graphite with mixed acid in a reactor, then adding an intercalator and stirring to react, and filtering, washing and drying to obtain layered graphite; then after microwave treatment of the layered graphite, dispersing the layered graphite in water for ultrasonic exfoliation to form a graphene aqueous liquid, and dispersing the centrifugalized graphene aqueous liquid in a solvent to obtain a graphene dispersion liquid; and then after ultrasonic treatment of the graphene dispersion liquid, forming a graphene thin film by virtue of dispensing or filtration of a cellulose filter membrane and polishing the surface of the graphene thin film, and furthermore, transferring the substrate and heating the graphene thin film to prepare the graphene conductive film. The preparation method is simple and convenient to operate, the controllability of process parameters is high and the production cost is low, and moreover, strong oxidants and toxic reducers are avoided, and the preparation method is environment-friendly.

Description

Technical field: [0001] The invention belongs to the technical field of graphene material preparation and relates to a method for preparing a high-quality graphene conductive film. Background technique: [0002] Graphene is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. In 2004, scientists at the University of Manchester in the United Kingdom stripped graphene for the first time and confirmed that it can exist stably. Since then, graphene, a new type of material, has received widespread attention. Graphene has very excellent properties, and its specific surface area is as high as 2630m 2 .g -1 , sign mobility up to 200000cm 2 .v -1 .s -1 , Young's modulus up to 1.0TPa, thermal conductivity constant of 5000W.m -1 .K -1 , the optical transmittance is as high as 97.7%, and its conductivity is also very good, almost reaching the conductivity of a s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 宗成中刘睿宗迎夏王春芙
Owner QINGDAO UNIV OF SCI & TECH
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