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Electrochemical preparation method of graphene

A graphene and electrochemical technology, applied in the field of electrochemical preparation of graphene, can solve the problems of slow chemical preparation process, high quality of graphene without impurities, high preparation cost and difficulty, and achieve low preparation cost and difficulty, and low price Low cost and low power consumption

Active Publication Date: 2015-05-06
SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The chemical method has mild reaction conditions, is easy to control, is suitable for the large-scale preparation of graphene, and has strong advantages in subsequent processing. Many existing research works are also based on this method, but the chemical method is slow and efficient. Low, and it is necessary to add toxic substances such as hydrazine hydrate, sodium borohydride, hydroquinone, etc., while the electroreduction method is to obtain electrons from the oxygen-containing functional groups on the oxidized graphene to be reduced, no toxic chemical reagents are involved, and the preparation method Simple, easy to control the reaction process, low cost, no pollution, and the prepared graphene has no impurities and high quality. It is a simple, green and large-scale production method for graphene
[0004] At present, the traditional method of preparing graphene by electroreduction of graphene oxide often requires high voltage to activate the reduction reaction, and the preparation of cumbersome and corrosive acidic solution or buffer solution as electrolyte is required, and the preparation cost and difficulty are high.

Method used

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preparation example Construction

[0024] Such as figure 1 The electrochemical preparation method of the graphene of one embodiment shown, comprises the steps:

[0025] S10, providing an electrode with electrocatalysis, and performing pretreatment on the electrode with electrocatalysis.

[0026] The surface of the electrode with electrocatalysis is provided with a coating with catalytic deoxidation effect. Specifically, the electrode with electrocatalysis can be an electrodeposited copper modified glassy carbon electrode, an electrodeposited nickel modified glassy carbon electrode or an electrodeposited copper nickel modified glassy carbon electrode.

[0027] Alternatively, the material of the electrode with electrocatalysis has a catalytic deoxygenation effect. Specifically, the electrode with electrocatalysis can be a copper electrode, a nickel electrode or a copper-nickel alloy electrode. The operation for pretreatment of the electrode is as follows: the electrode with electrocatalysis is polished and pol...

Embodiment 1

[0039] The graphene oxide prepared by the Modified Hummers method was dispersed in water, and peeled off in a 500W ultrasonic device for 2 hours to obtain a graphene oxide solution with a concentration of 1.2 mg / mL.

[0040] A copper electrode with a diameter of 3 mm was polished and polished with aluminum oxide with a particle size of 50 nm to 0.3 μm, and then ultrasonically cleaned with ethanol and distilled water to complete the pretreatment of the copper electrode.

[0041] 6 μL of a graphene oxide solution with a concentration of 1.2 mg / mL was dropped onto the surface of the pretreated copper electrode, and then the copper electrode was dried at room temperature to obtain a graphene oxide-modified copper electrode.

[0042] The graphene oxide-modified copper electrode was immersed in 0.1mol / L Na 2 SO 4 solution, and then perform a linear voltammetric sweep over the potential range of 0 to -1.5V. A cathodic current was evident at a potential of -0.7V and peaked at -1.2V....

Embodiment 2

[0044] The graphene oxide prepared by the Modified Hummers method was dispersed in water, and peeled off in a 500W ultrasonic device for 2 hours to obtain a graphene oxide solution with a concentration of 1.2 mg / mL.

[0045] A glassy carbon electrode with a diameter of 3 mm was polished by alumina with a particle size of 50 nm to 0.3 μm, and then ultrasonically cleaned with ethanol and distilled water.

[0046] Immerse the glassy carbon electrode in 0.5mol / L CuSO 4 In the solution, copper is electrodeposited in the range of 0V to -0.6V to obtain a copper-modified glassy carbon electrode.

[0047] 6 μL of graphene oxide solution with a concentration of 1.2 mg / mL was dropped onto the surface of the copper-modified glassy carbon electrode, and then dried at room temperature to obtain a graphene oxide-copper-modified glassy carbon electrode.

[0048] Immerse the graphene oxide-copper modified glassy carbon electrode in 0.1mol / L Na 2 SO 4In the solution, a linear voltammetry swe...

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Abstract

The invention discloses an electrochemical preparation method of graphene. The preparation method comprises the following steps: providing an electrode with the electrolysis action, and pretreating the electrode with the electrocatalysis action; dropping a graphene oxide solution onto the surface of the pretreated electrode with the electrocatalysis action, and drying to obtain a graphene oxide modified electrode; and soaking the graphene oxide modified electrode into a 10mmol / L-500mmol / L salt solution with the pH value of 7, regulating the potential of the electrode to be -1.2V to -2V and reacting for 1s to 1h, so as to obtain needed graphene. According to the electrochemical preparation method of the graphene, by matching the electrode with the electrocatalysis action with the salt solution with the pH value of 7 for use, the reduction action of graphene oxide can be activated with relatively low voltage, the neutral salt solution is green, simple to prepare, and low in price. Compared with a traditional electrochemical preparation method of the graphene, the electrochemical preparation method of the graphene is lower in preparation cost and difficulty.

Description

technical field [0001] The invention relates to an electrochemical preparation method of graphene. Background technique [0002] Graphene is a single-layer sheet structure composed of carbon atoms arranged in a honeycomb order. Graphene has excellent electrical, thermal and mechanical properties due to its unique structure, and is expected to be widely used in high-performance nanoelectronic devices, sensors, nanocomposites, batteries and supercapacitors, and field emission materials. Therefore, graphene, which only appeared in 2004, has rapidly become a research hotspot in physics, chemistry and materials science in recent years. [0003] The preparation of graphene is the basis of theoretical research and application research of graphene. At present, the electrochemical preparation methods of graphene mainly include mechanical exfoliation method, epitaxial growth method, chemical vapor deposition (CVD), chemical redox method, and liquid phase exfoliation method. Wait. A...

Claims

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Application Information

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IPC IPC(8): C25B1/00
CPCC25B1/00
Inventor 孙蓉张玲符显珠
Owner SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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