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Graphene film preparing method

A technology of graphene film and graphene powder, which is applied in the field of large-scale production of film preparation, can solve the problems of incapable of large-scale production, difficulty in film transfer, inability to continuous production, etc., and achieve good social and economic benefits, film thickness And the effect of controllable layer spacing and great commercial application prospects

Inactive Publication Date: 2016-01-06
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is only suitable for the preparation of single-layer or few-layer graphene films, and there are still many problems in this method, such as high cost, complicated process, inability to continuous production, and difficulty in film transfer.
When preparing graphene oxide and graphene film by suction filtration, graphene oxide is easy to block after film formation, which makes the film production process time-consuming, low efficiency, and thin film thickness, which is not suitable for industrial production
Other methods such as: spin coating, dipping, etc. also have problems such as not being able to scale production

Method used

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Experimental program
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Effect test

Embodiment 1

[0032] 1) Preparation of graphite oxide:

[0033] Get 10g (325 orders) natural flake graphite and 500ml mass concentration be 98% sulfuric acid after mixing uniformly, add 10.0g potassium nitrate, add 60g potassium permanganate rapidly in the water bath of 15 ℃, mix uniformly. Then the temperature of the system was raised to 40°C, reacted for 3h, then added 300ml of water, and simultaneously the system was heated to 80°C for 30min, then the excess potassium permanganate was reduced with 500ml of distilled water and 100ml of hydrogen peroxide (30wt%), and centrifugally washed to The pH is 5, diluted to a certain concentration, 100kHz ultrasonic for 2 hours to obtain a graphene oxide aqueous solution, and freeze-dried to obtain a graphene oxide powder.

[0034] 2) preparation of graphene oxide solution:

[0035] The powder of 1) was dispersed in formamide to form a 10 g / L graphene oxide suspension, and ultrasonicated at 100 kHz for 1 h to obtain a graphene oxide solution.

[0...

Embodiment 2

[0042] 1) Preparation of graphene oxide solution:

[0043] The graphene oxide powder was dispersed in water to prepare a 2 g / L graphene oxide suspension, and ultrasonicated at 40 kHz for 10 min to obtain a graphene oxide aqueous solution.

[0044] 2) Preparation of graphene oxide film

[0045] Take the solution of 1) and add it into the polytetrafluoroethylene ark, and the liquid level is 10cm high. The polytetrafluoroethylene ark was placed at 40°C to evaporate the solvent to obtain an ordered graphene oxide film.

[0046] 3) Preparation of graphene film

[0047] The film obtained in 2) was reduced in a nitrogen atmosphere at 500° C. for 120 min to obtain a graphene film.

[0048] figure 1 It is a cross-sectional view of the film structure. It can be seen from the figure that the layered microstructure of the film is flat and orderly, and the film thickness is 15um. figure 2 is the XRD pattern of the film, from the peak diffraction angle in the figure, the interlayer sp...

Embodiment 3

[0050] 1) Preparation of graphene oxide solution:

[0051] The graphene oxide powder was dispersed in a mixture of tetrahydrofuran and dimethyl sulfoxide (3:2) to form a 5 g / L graphene oxide suspension, and ultrasonicated at 80 kHz for 80 min to obtain a graphene oxide aqueous solution.

[0052] 2) Preparation of graphene oxide film

[0053] Take the solution of 1) and put it into the nylon-based container, and the liquid level is 20cm high. Place it at 80°C to volatilize the solvent to obtain an ordered graphene oxide film.

[0054] 3) Preparation of graphene film

[0055] The film obtained in 2) was reduced in a nitrogen atmosphere at 800° C. for 60 min to obtain a graphene film.

[0056] The interlayer spacing of the film was measured as The film thickness is 23um, and the contact angle is 87.76°.

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Abstract

The invention relates to a graphene film preparing method. The preparing method includes the steps that oxidized graphene is dispersed in solvent, a highly-ordered oxidized graphene film of a three-dimensional layered structure is built through a solvent evaporation method, the distance between film layers is controlled by adjusting and controlling evaporation speed through control over evaporation temperature, and then a graphene film with controllable layer structures and different hydrophilicity and hydrophobicity is obtained through reduction. The characteristics of surface functional groups as well as hydrophilicity and hydrophobicity of oxidized graphene and graphene are combined innovatively, the film is formed fast in suitable solvent by regulating and controlling evaporation speed, the advantages of the controllable structure, high orderliness and adjustable thickness of the film are achieved, and the oxidized graphene and graphene film preparing method is easy to operate, low in cost and free of pollution. The problems that a CVD method for growing the graphene film is high in cost and cannot be scaled up are solved, the bottleneck problems that a suction filtration method and the like for preparing the oxidized graphene and graphene films take long time, and the films are thin are solved, and the graphene film preparing method has huge industrialization prospects.

Description

Technical field: [0001] The invention relates to a preparation method of a graphene film, which belongs to a film preparation method which is fast and effective, has adjustable thickness, controllable layer structure and is suitable for large-scale production. Background technique: [0002] In recent years, graphene has gradually become a hot spot of international scientific research because of its special structure and properties. Graphene is a single layer of carbon atoms with sp 2 The hexagonal honeycomb lattice planar film composed of hybrid orbitals has a theoretical single-layer graphene thickness of 0.34nm; the theoretical specific surface area is about 2600m 2 / g; The connection between the carbon atoms inside graphene is very flexible. When an external force is applied to graphene, the surface of the carbon atoms will be bent and deformed, so that the carbon atoms do not have to be rearranged to adapt to the external force, so graphene also has strong mechanical pr...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 暴宁钟孙艳何大方沈丽明张晓艳
Owner NANJING UNIV OF TECH