Device and method for preparing graphene film on basis of plasma

A graphene thin film and plasma technology, applied in the field of energy storage materials, can solve the problems that hinder the large-scale preparation and application of high-quality nanomaterials, destroy the graphene sheet structure, and the plasma electron energy is large, and meet the thermal stability requirements of the equipment Low, reduce pollution and human health hazards, mild and controllable reaction conditions

Active Publication Date: 2015-06-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the energy of the above-mentioned plasma electrons is large, the reduction process will destroy the graphene sheet structure, and the requirements for the emission source are high, which hinders the large-scale preparation and application of this high-quality nanomaterial to a certain extent.

Method used

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  • Device and method for preparing graphene film on basis of plasma
  • Device and method for preparing graphene film on basis of plasma
  • Device and method for preparing graphene film on basis of plasma

Examples

Experimental program
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Effect test

preparation example Construction

[0035] 2) Preparation of graphene oxide film: ultrasonically disperse the graphene oxide prepared in step 1) in deionized water to obtain a uniformly dispersed graphene oxide solution, which is filtered through a microporous membrane with a pore size of 0.22 microns and dried. Tear off the graphene oxide film from the microporous membrane for subsequent use;

[0036]3) Put the graphene oxide film prepared in step 2) on the sample support frame 5, turn on the vacuum pump 8 and the gas regulating valve 1, pass inert gas into the quartz tube 7, and adjust the flow rate of the inert gas with the mass flow meter 2 to 7-10 ml / min, rotate the vacuum regulating valve 9, and adjust the air pressure in the quartz tube 7 to 250-320 millitorr;

[0037] 4) Keep the air pressure and gas flow in the quartz tube 7 constant, turn on the high-voltage negative power supply 3, adjust the voltage to 7-10 kV, and form a stable glow discharge plasma between the cathode electrode 4 and the anode elec...

Embodiment 1

[0043] 1. Modified Hummers oxidation method to prepare graphene oxide: natural flaky graphite and concentrated sulfuric acid (mass concentration 98%) were stirred evenly at room temperature, wherein the mixing ratio of concentrated sulfuric acid and natural flaky graphite was 25 mg: 1 gram, and the mixture was placed in an ice bath After dropping to 0 oC, slowly add potassium permanganate to it and mix evenly with magnetic stirring, wherein the quality of potassium permanganate is 3.5 times that of natural flake graphite. Cool down, then add deionized water and hydrogen peroxide in sequence, wherein the ratio of deionized water to natural flake graphite is 100 ml: 1 g, and the ratio of peroxidized to natural flake graphite is 8 ml: 1 g, the mixed solution Repeated cleaning treatment by high-speed centrifugation, placed in the air, and dried at room temperature to obtain graphene oxide.

[0044] 2. Preparation of graphene oxide film: ultrasonically disperse the graphene oxide...

Embodiment 2

[0052] Repeat Example 1, the only changes in the working conditions are: the distance between the cathode and anode plates is 80 mm, the distance between the cathode plate and the sample is 60 mm, and the distance between the anode plate and the sample is 20 mm, that is, the distance ratio between the cathode electrode, the anode electrode and the sample support frame 3, the inert gas is helium, the helium gas flow rate is 10 ml / min, the DC high voltage negative power supply voltage is 7 kV, and the reaction lasts for 1 minute. The carbon-oxygen atomic ratio of the graphene film obtained above is 6.5, and the peak intensity ratio of the D peak and the G peak is 1.06.

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PUM

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Abstract

The invention discloses a device and a method for preparing a graphene film on basis of plasma. According to the device, a sample support frame is horizontally arranged in the middle of a quartz tube, a negative electrode is arranged at the upper part of the quartz tube, a positive electrode is arranged at the lower part of the quartz tube, sealing rubber plugs are arranged at the upper and lower ends of the quartz tube, a negative glow zone is arranged between the negative electrode and the sample support frame, a Faraday dark space is arranged between the positive electrode and the sample support frame, a gas regulating valve is connected with the upper part of the quartz tube through a mass flowmeter and the sealing rubber plug at the upper end, a high-voltage negative power supply is connected with a negative electrode through the sealing rubber plug at the upper end, a vacuum pump is connected with the lower part of the quartz tube through a vacuum regulating valve, a vacuometer and the sealing rubber plug at the lower end, and the positive electrode is grounded through the sealing rubber plug at the lower end. The graphene film prepared in the invention is high in degree of graphitization and has excellent properties; in addition, compared with the traditional chemical reduction method and thermal reduction method, the preparation method disclosed by the invention has the advantages of short time consumption, high reduction efficiency, no need of a reducing agent or heating source and the like and has a potential for large-scale industrial application.

Description

technical field [0001] The invention belongs to the technical field of energy storage materials, and in particular relates to a device and method for preparing graphene thin films based on plasma. Background technique [0002] Graphene is composed of a layer of carbon atoms with sp 2 The hexagonal lattice material composed of hybrid orbitals is the thinnest two-dimensional material found so far. Since it was first successfully exfoliated from graphite crystals by Geim, a scientist at the University of Manchester in the United Kingdom, in 2004, graphene materials are due to It has high strength (125 GPa), good thermal conductivity (about 5000W / (m?K)), excellent carrier mobility (200000 cm 2 / (V?s)) and large specific surface area (theoretical value 2630 m 2 / g), etc., have shown broad application prospects in the fields of electronics, information, energy, and composite materials, and have greatly promoted the large-scale and batch preparation technology of high-quality gra...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 薄拯岑可法严建华池涌李晓东钱佳静
Owner ZHEJIANG UNIV
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