Electrochemistry stripping and reducing integrated graphene preparation method

A graphene and electrochemical technology, which is applied in the field of graphene preparation integrating electrochemical exfoliation and reduction, can solve the problem that graphene oxide sheets are folded into worm-like shapes, the lateral sizes of graphene are different, and the graphene preparation process is cumbersome. Complexity and other problems, to achieve the effect of low cost of raw materials, low cost and easy operation

Inactive Publication Date: 2013-03-13
TONGJI UNIV
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Problems solved by technology

[0003] Among them, the exfoliation of graphite oxide (GO) is a key step in the whole redox process. Common exfoliation methods include ultrasonic and pyrolytic expansion exfoliation. Ultrasonic exfoliation not only has noise pollution, but also the obtained graphene has different lateral sizes; thermal The peeling yield of the deswelling peeling method is not high, it is easy to cause the graphene oxide sheet to fold into a worm shape, and the requirements for the equipment are relatively high
Reduction is the core step in the whole redox process, which can be obtained by reducing graphene oxide with heat, light or electric field. The thermal reduction method will destroy the structure of graphene. In addition, it has higher requirements on equipment and environment. ; The thickness of graphene sheet obtained by photocatalytic reduction method is relatively thick, which will limit its performance and application
Not only there are some problems in the existing exfoliation and reduction methods, but also the separate study of them also makes the preparation process of graphene cumbersome and complicated, which is not conducive to popularization and use. Therefore, an efficient, environmentally friendly experimental method that can simultaneously complete the exfoliation and reduction is sought It is very important, especially in electrochemistry to realize the process with alternating field, which has not been reported yet. The present invention combines the basic principles of electrochemistry and the concept of green chemistry, and proposes the following simple, efficient and environmentally friendly alternating field stripping Reduction method, the test results prove that the graphene prepared by this method has good peeling and reduction effects and high quality

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  • Electrochemistry stripping and reducing integrated graphene preparation method

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Embodiment 1

[0032] The device of this embodiment is as figure 1 As shown, the signal generator 1 is connected to the power amplifier 2, and the power amplifier 2 is connected to the electrode 4, wherein the power amplifier 2 is connected to the oscilloscope 3 that detects the frequency and waveform of the electrical signal at the same time, and the graphite oxide aqueous solution 5 is applied to the alternating current through the signal generator 1. electric field.

[0033] The reaction time of the present embodiment is 120 minutes.

[0034] First, 30 μm natural graphite was used as raw material to prepare GO by the improved hummers method; the obtained GO was dissolved in deionized water to prepare a 0.2 mg / ml GO suspension; a self-made electrochemical reaction glass container (length 4 cm, width 2 cm, height 10 cm ) and two copper electrodes (3.5cm in width and 10cm in length), insert the two copper electrodes into the glass container with a distance of 2cm between the two electrodes,...

Embodiment 2

[0039] The device of this embodiment is as figure 1 Shown, reaction time 90 minutes.

[0040] First, 30 μm natural graphite was used as raw material to prepare GO by the improved hummers method; the obtained GO was dissolved in deionized water to prepare a 0.2 mg / ml GO suspension; a self-made electrochemical reaction glass container (length 4 cm, width 2 cm, height 10 cm ) and two copper electrodes (3.5cm in width and 10cm in length), insert the two copper electrodes into the glass container with a distance of 2cm between the two electrodes; 0.5Hz, duty cycle 20%, voltage 40V); pour 50ml of the prepared GO suspension into a glass container, turn on the power, stop the reaction after 90 minutes of reaction, and obtain high-quality rGO;

[0041] The obtained rGO was analyzed by atomic force microscope, infrared spectrum and X-ray diffraction to verify its reduction. The results are as follows: Figure 5 , Figure 6 and Figure 7 shown.

[0042] From Figure 5 It can be see...

Embodiment 3

[0046] A kind of graphene preparation method of electrochemical exfoliation and reduction integration, the method comprises the following steps:

[0047] (1) Dissolve graphite oxide in deionized water to form a graphite oxide solution with a concentration range of 0.1 mg / ml;

[0048] (2) graphite oxide solution is added in the reaction vessel, and the reaction vessel can be a glass or plastic container;

[0049] (3) applying an alternating electric field in the graphite oxide solution;

[0050] (4) Graphite oxide reacts electrochemically in the environment of alternating electric field to generate graphene.

[0051] The method of applying the alternating electric field in step (3) is as follows: the signal generator outputs the signal, and the signal is input into the power amplifier. Frequency, output the amplified electrical signal to the electrode, that is, an alternating electric field is obtained. The distance between the two electrodes is 0.5cm, the electrodes are cop...

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Abstract

The invention relates to an electrochemistry stripping and reducing integrated graphene preparation method. The method comprises the following steps of: (1) taking graphite oxide and dissolving the graphite oxide in deionized water so as to prepare a graphite oxide solution with a concentration range of 0.1-1mg / ml; (2) adding the graphite oxide solution into a reaction container; (3) applying an alternating electric field to the graphite oxide solution; and (4) generating an electrochemistry reaction via the graphite oxide in the environment of the alternating electric field so as to generate the graphene. Compared with the prior art, the method provided by the invention has the following beneficial effects: the principle of the electrochemistry reduction and the excellent electrochemistry property of the graphene are effectively combined, so that the defects existing in other preparation methods are overcome; and the electrochemistry stripping and reducing integrated graphene preparation method not only can be used for realizing a graphene preparing method with integrated stripping and reducing, but also has the advantages of simplicity in operation, low cost, safety, no pollution and the like.

Description

technical field [0001] The invention relates to a preparation method of graphene, in particular to a preparation method of graphene integrating electrochemical exfoliation and reduction. Background technique [0002] Graphene (rGO) is a layer of carbon atoms with a thickness of one atom. Since its appearance in 2004, it has attracted extensive attention in many fields. Because of their unique physical and chemical properties, they have shown great potential in optics, sensing, catalysis, and electronics. Wide application prospects in other fields. Existing graphene preparation methods include mechanical exfoliation, epitaxial growth, vapor deposition, and redox methods. The oxidation-reduction method is a preparation method of oxidizing, exfoliating, and reducing graphite. This method is simple to operate and low in cost. So far, it is considered to be the most economical method for producing and preparing graphene. [0003] Among them, the exfoliation of graphite oxide (G...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/192
Inventor 张东刘艳云郭超
Owner TONGJI UNIV
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