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A method for preparing graphene film by microwave combined with sol-gel process

A technology of graphene film and sol, which is applied in the field of nanomaterials, can solve problems such as the influence of film conductivity, complicated process, and the performance of graphene film, and achieve the effects of easy control, simple process, excellent thermal conductivity and hydrophobicity

Active Publication Date: 2021-05-25
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are many common methods for preparing graphene films. For example, Chen et al. prepared graphene films by the two-phase interface method. Inject ethanol, and self-assemble at the liquid-gas interface to form a uniform and transparent graphene oxide film through the double-driven action of non-aqueous solvent ethanol and n-pentane; the film formed by this method is easy to transfer to a solid support, but due to Graphene oxide is used as a raw material. Although it is subsequently reduced, there are still a large number of defects on the surface of graphene, which have a certain impact on the conductivity of the film.
Kim et al. prepared graphene film by template method. Firstly, the modified silicon dioxide sheet was immersed in the aminated carbon nanotube solution, and then thermally reduced to obtain a graphene-carbon nanotube film. The film has good light transmittance. ; but the process is complicated, and the removal of the template will have a certain impact on the properties of the graphene film

Method used

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  • A method for preparing graphene film by microwave combined with sol-gel process
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  • A method for preparing graphene film by microwave combined with sol-gel process

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Effect test

Embodiment 1

[0036]Put 0.2 g of flake graphite powder into a microwave oven, and use 350W power microwave to expand for 30 minutes to obtain expanded flake graphite powder. Mixed dibasic acid ester (DBE) was selected as the solvent, and dimethylamine was used as the intercalation agent. Take 0.2g of expanded graphite powder, add 200mL of mixed dibasic acid ester (DBE) and 15mL of dimethylamine, and process at 40KHz ultrasonic frequency for 240min to obtain graphene sol, aging at room temperature for 12h, and coating on glass substrate by dipping and pulling , and finally dried at 60°C for 6h to prepare a graphene film. The thickness of the graphene film was measured to be 20.5 μm. The measured wetting angle of the film is 110.6°, as Figure 4 shown.

Embodiment 2

[0038] Put 0.2 g of flake graphite powder into a microwave oven, and expand it for 3 minutes by using a microwave with a power of 3000W to obtain expanded flake graphite powder. Ethyl acetate was selected as the solvent, and monomethylamine was used as the intercalation agent. Take 0.2g of expanded graphite powder, add 100mL of ethyl acetate and 3mL of monomethylamine, and process it at an ultrasonic frequency of 25KHz for 360min to obtain a graphene sol, age at 80 for 2h, immerse the melamine foam in the sol for 2h, remove the sol, and finally Dry at 80°C for 4 hours to prepare a graphene film. The measured wetting angle of the film is 137°, as Figure 5 shown.

Embodiment 3

[0040] Put 0.2 g of flake graphite powder into a microwave oven, and use 1000W power microwave to expand for 10 minutes to obtain expanded flake graphite powder. Methyl acetate was selected as the solvent, and diethanolamine was used as the intercalation agent. Take 0.2g of expanded graphite powder, add 80mL of ethyl acetate and 12mL of monomethylamine, and process it at an ultrasonic frequency of 68KHz for 30min to obtain a graphene sol, age at room temperature for 72h, immerse the melamine foam in the sol for 4h, remove the sol, and finally Dry at 40°C for 10 h to prepare a graphene film.

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Abstract

The invention relates to a method for preparing a graphene film by combining microwave with a sol-gel process. The method comprises: taking flake graphite powder as a raw material, obtaining expanded flake graphite powder after microwave treatment; using the obtained expanded flake graphite powder as Precursor, using small molecule amines as intercalation agent, after adding ester solvent, intercalation and stripping to form graphene sol; after aging the obtained graphene sol, forming a film on the substrate and drying, the graphite vinyl film. The process of the invention is characterized by no oxidation / reduction process, low cost of equipment and raw materials, simple process and easy control.

Description

technical field [0001] The invention belongs to the field of nanomaterials, and in particular relates to a method for preparing a graphene film by a novel microwave combined with a sol-gel process. Background technique [0002] Graphene is made of carbon atoms with sp 2 The hybrid forms link into a single atomic layer 2D material. Graphene has excellent thermal, mechanical, electrical and optical properties. At the same time, graphene film has many advantages, such as good electrical conductivity, high light transmittance, and strong hydrophobicity, so graphene is often used in light-emitting, display and other devices. In the fields of solar cell devices and DC electronic devices, especially when used as a transparent electrode, good device performance can be obtained, and the bending resistance of the device is also much stronger than that prepared by the ITO transparent electrode. Moreover, graphene films are expected to be widely used in displays, supercapacitors, fie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
CPCC01B2204/20C01B2204/22C01B2204/24C01P2004/61
Inventor 江峰于云宋力昕冯爱虎王勇于洋米乐
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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