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Method for preparing reduced graphene oxide by using dielectric barrier discharge plasma

A technology of dielectric barrier discharge and plasma, which is applied in the direction of graphene, single-layer graphene, chemical instruments and methods, etc., can solve the problems of less processing capacity, easy agglomeration, and low output, and achieve low resource and energy consumption, Prevent aggregation and re-growth, high production efficiency

Active Publication Date: 2018-02-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned methods have their own defects. For example, the reducing agent used in the chemical reduction method has the disadvantages of high pollution and high toxicity, and needs subsequent removal, which makes the operation complicated; the photocatalytic reduction method has a reaction cycle of more than 5 hours and requires light that is difficult to separate Catalyst: The electrochemical reduction method is carried out in a low-concentration graphene oxide dispersion of 0.1 to 5 mg / mL, with low processing capacity and high surface tension of graphene, which is prone to agglomeration, which is not conducive to the formation of reduced graphene with fewer layers; The thermal reduction method can directly reduce the graphene oxide powder in an inert atmosphere, but requires a higher temperature, is difficult to operate, requires high equipment requirements, and consumes a lot of energy.
[0004] Through relevant document retrieval, there is the report that a small amount of plasma treatment carbon material prepares graphene, for example, CN102153076A, CN104609408A, CN102781831A adopt plasma treatment graphite, CN101993060A adopt plasma treatment graphene oxide, but all adopt arc discharge thermal plasma, temperature reaches 4000-5000K high temperature, difficult operation, high equipment requirements, high energy consumption; using plasma polishing technology (CN103484889A) to process graphite in hot solution (60-95 ℃) to prepare graphene solution, but the obtained graphene is easily Agglomeration into particles is not conducive to application, and the resulting product needs subsequent treatment such as dilution, ultrasonication, washing, and drying, with a cycle of up to 7 hours; microwave plasma (CN102107870A), inductively coupled plasma (CN104085884A) or glow discharge plasma (CN103818899A) Processing graphene oxide to prepare graphene, complex equipment and less processing capacity
[0005] In addition, plasma can efficiently decompose methane, ethane, acetylene, ethanol, sucrose and other carbon source gases, and can assist chemical vapor deposition to prepare graphene, such as: CN105152165A, CN104773725A, CN103570006A, CN103183334A and CN103708444A, but this method The substrate needs to be placed in a high temperature zone of 300-1000°C and a low pressure of 10-1000Pa, the device is complex, the usage rate of reactants is low, and the output is low

Method used

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  • Method for preparing reduced graphene oxide by using dielectric barrier discharge plasma
  • Method for preparing reduced graphene oxide by using dielectric barrier discharge plasma
  • Method for preparing reduced graphene oxide by using dielectric barrier discharge plasma

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Experimental program
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Effect test

Embodiment 1

[0036] The multilayer graphene oxide powder prepared by the Improved method is placed between the two electrodes of the plate-plate dielectric barrier discharge device, and argon gas is passed in at room temperature (20-30°C) as the discharge gas, and the high-voltage power supply is turned on to adjust the working conditions. The voltage was 1000V, the working current was 1.0A, and the discharge treatment was performed at room temperature for 3 minutes. The obtained product was characterized and analyzed by XRD, TG, and XPS, which proved that graphene oxide was reduced. The carbon source conversion rate in the preparation process is 90%, and the specific surface area is 410m 2 / g. The characterization results are shown in figure 1 , 2 and 3.

Embodiment 2

[0038] Place the multilayer graphene oxide sheet prepared by the Staudenmaier method between the two electrodes of the plate-plate dielectric barrier discharge device, pass nitrogen gas as the discharge gas at room temperature (20-30°C), turn on the high-voltage power supply, and adjust the operating voltage To 500V, working current to 1.0A, discharge treatment at room temperature for 60min, the obtained product was analyzed by XRD and TG, which proved that graphene oxide was reduced. The conversion rate of carbon source in the preparation process is 96%, and the specific surface area is 467m 2 / g.

Embodiment 3

[0040] Place the single-layer graphene oxide powder prepared by the Hummers method between the two electrodes of the point-plate dielectric barrier discharge device, feed air at room temperature (20-30°C) as the discharge gas, turn on the high-voltage power supply, and adjust the working voltage To 1000V, working current to 1.0A, discharge treatment at room temperature for 60min, the obtained product was analyzed by XRD and TG, which proved that graphene oxide was reduced. The carbon source conversion rate in the preparation process is 92%, and the specific surface area is 489m 2 / g.

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Abstract

The invention relates to a method for preparing reduced graphene oxide by using dielectric barrier discharge plasma. The method comprises the following steps: (1) placing the graphene oxide between two electrodes in a plasma device; (2) introducing plasma discharge gas; (3) applying high voltage to the two electrodes, enabling the device to produce plasma, and treating for a period of time to obtain the finished product. The method is simple in equipment, simple and convenient to operate, low in energy consumption, free from pollution and high in production efficiency; furthermore, after the method is adopted, the carbon source conversion rate reaches up to 90% or above, and the specific surface area is increased to 400m <2> / g or more from about 100m<2> / g in the heat treatment reduction method; therefore, the method provided by the invention is a novel preparation method which is low in cost, easy to popularize and suitable for practical production.

Description

technical field [0001] The invention belongs to the technical field of graphene manufacturing process improvement, in particular to a method for preparing reduced graphene oxide by dielectric barrier discharge plasma. Background technique [0002] Graphene is made of carbon atoms with sp 2 Two-dimensional nanomaterials with hybrid orbitals arranged in a honeycomb lattice have good strength, flexibility, electrical conductivity, thermal conductivity, and optical properties. They are considered to be the next generation of microelectronic devices, organic photoelectric materials, and efficient storage It is the preferred material in the fields of energy materials, multifunctional composite materials and biomedicine. [0003] At present, the reduction of graphene oxide is considered to be the most feasible method for large-scale preparation of graphene, including chemical reduction, photocatalytic reduction, electrochemical reduction, and thermal reduction. The above-mentione...

Claims

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Application Information

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IPC IPC(8): C01B32/184
CPCC01B2204/02C01B2204/04C01B2204/32C01P2002/72C01P2002/88
Inventor 王召彭祥凤侯宝红郝红勋龚俊波王永莉鲍颖张美景尹秋响
Owner TIANJIN UNIV
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