Preparation method of graphene thin film

A graphene film, graphene technology, applied in the direction of graphene, nano-carbon, etc., can solve the problem of small size of graphene oxide and graphene powder, inability to further prepare graphene assembly, and high requirements for graphene size uniformity, etc. problems, to achieve the effect of reducing severe shrinkage and agglomeration, facilitating collection and avoiding damage

Active Publication Date: 2018-12-11
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the preparation process of the above-mentioned graphene film, graphene oxide is mostly used as raw material, but during the solvent volatilization process of the preparation process, the graphene oxide film is easy to shrink and agglomerate, resulting in incomplete surface of the film. If graphene is directly used as raw material , not only requires high uniformity of graphene size, but also graphene basically has no self-assembly ability in the preparation process
The most commonly used redox method uses graphite as raw material, which has the advantages of simple process, low cost, and large-scale production. However, the graphene oxide and graphene powder obtained by this method are small in size and easy to agglomerate, which is not easy application, it is not possible to further prepare large-scale graphene assemblies to regulate the properties of graphene and expand the application range of graphene

Method used

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Experimental program
Comparison scheme
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Embodiment 1

[0025] The preparation method of the present embodiment comprises the following steps:

[0026] Step 1, adding 0.1g graphene oxide to 1000mL mixed solvent, then stirring and dissolving under the condition of ultrasonic vibration to obtain a precursor solution; the concentration of graphene oxide in the precursor solution is 0.1mg / mL; the mixed solvent It is made by mixing 167mL water and 833mL ethanol;

[0027] Step 2, add 0.5g zinc flakes to the precursor solution obtained in step 1, then stir under the condition of ultraviolet light irradiation to carry out the reduction reaction, then stratify after standing, the upper layer solution obtained is a weakly reduced graphene colloid ;

[0028] Step 3, the weakly reduced graphene colloid that obtains in step 2 is coated on glass by spin coating method, obtains the weakly reduced graphene thin film that is attached to glass surface; The spin coating speed that described spin coating method adopts is 500 revolutions / minutes, th...

Embodiment 2

[0033] The preparation method of the present embodiment comprises the following steps:

[0034] Step 1, 1g graphene oxide is added in 1000mL mixed solvent, then stir and dissolve under the condition of ultrasonic vibration, obtain precursor solution; The concentration of graphene oxide in the described precursor solution is 1mg / mL; Described mixed solvent is made up of 375mL Water mixed with 625mL ethanol;

[0035] Step 2, adding 5g Ti6Al4V sheets to the precursor solution obtained in step 1, then stirring and carrying out the reduction reaction under the condition of ultraviolet light irradiation, and then stratifying after standing, the upper layer solution obtained is a weakly reduced graphene colloid;

[0036] Step 3, the weakly reduced graphene colloid obtained in step 2 is coated on the Si sheet by the spin coating method to obtain a weakly reduced graphene film attached to the surface of the Si sheet; the spin coating speed adopted by the spin coating method is 1500 rev...

Embodiment 3

[0040] The preparation method of the present embodiment comprises the following steps:

[0041] Step 1, 2g graphene oxide is added in 1000mL mixed solvent, then stir and dissolve under the condition of ultrasonic vibration, obtain precursor solution; The concentration of graphene oxide in the described precursor solution is 2mg / mL; Described mixed solvent is made of 500mL Water mixed with 500mL methanol;

[0042] Step 2: Add 10g of spherical particle Cu to the precursor solution obtained in step 1, then stir and carry out the reduction reaction under the condition of ultraviolet light irradiation, and then stratify after standing, the upper layer solution obtained is a weakly reduced graphene colloid ;

[0043] Step 3, the weakly reduced graphene colloid obtained in step 2 is coated on the microporous membrane by vacuum filtration method, and the weakly reduced graphene film attached to the bottom surface of the microporous membrane is obtained;

[0044] Step 4, place the we...

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PUM

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Abstract

The invention discloses a preparation method of a graphene thin film. The preparation method comprises the following steps: 1, adding graphene oxide into a mixed solvent and dissolving to obtain a precursor solution; 2, adding metal into the precursor solution and carrying out photocatalytic weak reduction reaction; after standing, layering to obtain weakly-reduced graphene colloid; 3, coating a substrate with the weakly-reduced graphene colloid to obtain a weakly-reduced graphene thin film attached on the surface of the substrate; 4, reducing the weakly-reduced graphene thin film attached onthe surface of the substrate and drying to obtain the graphene thin film. According to the preparation method disclosed by the invention, graphite oxide is weakly photocatalytically reduced into weakly-reduced graphene and then the weakly-reduced graphene is reduced into the graphene thin film; part of oxygen-containing groups are also remained on the weakly-reduced graphene, so that the graphenethin film has a self-assembling capability and the orderliness of the weakly-reduced graphene colloid is ensured; the quality of the graphene thin film is improved, the shrinkage and agglomeration ofthe graphene thin film in a drying process are reduced, damages to the graphene thin film are avoided and a size range of the graphene thin film is expanded.

Description

technical field [0001] The invention belongs to the technical field of graphene material preparation, in particular to a method for preparing a graphene film. Background technique [0002] Graphene is a hexagonal close-packed two-dimensional crystal composed of a single layer of carbon atoms. It has the advantages of high electrical conductivity, high light transmittance, excellent mechanical strength and chemical stability. Therefore, graphene two-dimensional assembled film is widely used in the field of electronic devices. , nanofiltration membrane and other fields have broad application prospects. [0003] At present, researchers can use a variety of methods to prepare high-quality graphene, such as mechanical exfoliation, redox, chemical vapor deposition, crystal epitaxial growth, etc., and then use suction filtration, spin coating, spray coating , LB film method, etc. to prepare graphene into graphene paper or film. In the preparation process of the above-mentioned gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B32/184
Inventor 金利华白利峰刘国庆冯建情李成山张平祥
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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