Preparation method of large-area reduced graphene oxide membrane

A graphene film, a large-area technology, applied in the field of large-area reduced graphene oxide film preparation, can solve the problems of layered structure density reduction, large-area integrity damage, affecting mechanical properties and applications, etc., to achieve size and The effect of controllable structure and low cost

Active Publication Date: 2016-08-24
王祉豫
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Problems solved by technology

However, the thermal reduction method has not been able to effectively and continuously prepare large-area and high-quality reduced graphene oxide films. The primary limiting factor is: thermally reduced graphene oxide films usually need to be heated slowly in a protective atmosphere to ensure that their sheets The structure is stable, and rapid heating and reduction will lead to the rapid defunctionalization of graphene oxide and the release of a large amount of gas, which will cause the internal pressure of the membrane to increase sharply, resulting in the destruction of the integrity of the large area of ​​the membrane and the large increase in the density of the layered structure. reduced, thus seriously affecting its mechanical properties and applications

Method used

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  • Preparation method of large-area reduced graphene oxide membrane

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preparation example Construction

[0026] A kind of preparation method of large-area reduced graphene oxide film of the present invention comprises the following steps:

[0027] (1) Using graphite powder as a raw material to prepare a suspension of graphene oxide;

[0028] (2) Evenly disperse the suspension of graphene oxide on the surface of the substrate by spraying or scraping to form a graphene oxide film;

[0029] (3) Reducing the graphene oxide film under hot rolling conditions to obtain a reduced graphene oxide film.

[0030] In the step (1), the graphene oxide suspension is a deionized water phase suspension, or an organic phase suspension, and the concentrations of the deionized water phase suspension and the organic phase suspension are controlled at 1-30mg / mL, the organic solvents include ethanol (ethanol), dimethylformamide (DMF), N-methylpyrrolidone (NMP), tetrahydrofuran (THF), dimethyl sulfoxide (DMSO), acetone (Acetone) or Isopropyl alcohol (IPA).

[0031] In the step (1), the graphene oxide...

Embodiment 1

[0047] A kind of preparation method of large-area reduced graphene oxide film of embodiment 1, preparation steps are:

[0048] (1) Graphene oxide was prepared by the improved Hummers method, the specific steps were: mix 6g graphite powder with 5g K 2 S 2 o 8 and 5g P 2 o 5 were added to 25mL of concentrated sulfuric acid at 80°C for pretreatment, and then the pretreated graphite was mixed with 30g KMnO 4 Add together to 230mL of concentrated sulfuric acid for further oxidation, then add 25mL of 30% hydrogen peroxide to the solution and wash with 2L of 10% dilute hydrochloric acid to obtain graphite oxide; dialyze the graphite oxide with deionized water to remove the remaining acid and salt until the pH value of the dialysate is 6-7; the graphite oxide is mechanically peeled off with a probe ultrasonic at a power of 150W for 1 hour, and the graphene oxide solution is centrifuged at 3000rpm with a rotary centrifuge, and Separating the upper layer solution to obtain a suspen...

Embodiment 2

[0051] A method for preparing a large-area reduced graphene oxide film in Example 2, the preparation steps (1) and (2) are the same as the steps (1) and (2) of Example 1; the preparation step (3) is: the oxidation The graphene film is sandwiched between two 60cm×20cm copper foils; adjust the pressure of the hot roll and the lower plate to 10MPa, and raise the temperature of the hot roll to 600°C, and then place the graphene oxide film protected by the copper foil at 20cm / The speed of min is to carry out hot rolling reduction treatment by hot rolling, and the reduced graphene oxide film is exported and separated from the copper foil, such as figure 1 shown.

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Abstract

The invention relates to a method for preparing a large-area reduced graphene oxide membrane. The method comprises the preparation steps that graphite powder serves as the raw material to prepare a graphene oxide suspension; the graphene oxide suspension is uniformly dispersed on the surface of a substrate in a spray coating or blade coating mode, and a graphene oxide membrane is prepared; the graphene oxide membrane is subjected to reduction treatment under the hot rolling condition, and the reduced graphene oxide membrane is obtained. According to the method for preparing the large-area reduced graphene oxide membrane, rapid heat treatment is conducted under the hot rolling condition, and therefore continuous preparation of the large-area reduced graphene oxide membrane is achieved. The method is convenient to operate, the process is simple and flexible, the production cost of the reduced graphene oxide membrane is greatly reduced, the production efficiency is improved, and the method is suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of large-area two-dimensional material film preparation, in particular to a method for preparing a large-area reduced graphene oxide film. Background technique [0002] The discovery and application of new materials determine the innovation and breakthrough of human beings in the use of tools. In recent years, due to the discovery of a series of carbon nanomaterials, people predicted the coming of an era of new functional materials - carbon materials. Among them, graphene has attracted widespread attention in the field of science and technology all over the world as soon as it came out. This discovery also won the Nobel Prize in Physics in 2010. Graphene is a single layer of carbon atoms with SP 2 The hexagonal honeycomb lattice composed of hybrid orbitals is a two-dimensional material. Graphene theoretically has excellent electrical, thermal, chemical and mechanical properties. Its potential applications ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 王祉豫
Owner 王祉豫
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