Preparation method of graphene

A technology of graphene and graphite, which is applied in the field of two-dimensional nanomaterials and its preparation, can solve the problems of complex operation process, high toxicity and high production cost, and achieve the effect of wide application prospect, less impurity elements and excellent performance

Active Publication Date: 2013-01-09
苏州汇涵医用科技发展有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] At present, the preparation methods of graphene mainly include: mechanical exfoliation method (K.S.Novoselov, et al, Science, 2004, 306, 666-669), chemical vapor deposition method (A. Reina, et al, Nano Lett., 2009, 9, 30-35), epitaxial growth method (P.W.Sutter, et al, Nat. Mater., 2008, 7, 406-411), chemical redox method (D.Li, et al, Nat. Nanotechnol., 2008, 3, 101-105); these methods have their own advantages and disadvantages. The graphene obtained by mechanical exfoliation has high purity and good conductivity, but the yield is low and the mixed product of graphene is difficult to obtain. Separation; high-quality, large-area graphene can be prepared by chemical vapor deposition, and single-layer graphene can be prepared by epitaxial growth, but these two methods require high temperature and high pressure, harsh experimental conditions, complex operating processes, and high production costs ; Compared with the first three methods, the chemical redox method has the advantages of simple operation process, mild experimental conditions, and low production cost, and is more suitable for large-scale production
[0004] The reducing agent of graphene prepared by the chemical reduction of graphene oxide reported in current literature mainly contains: hydrazine hydrate (Stankovich S, et al, J Mater Chem, 2006,16,155- 158), hydroquinone (G.X.Wang, et al, Carbon, 2009, 47, 1359-1364) and sodium borohydride (J.F.Shen, et al, Chem. Mater., 2009, 21, 3514-3520), etc.; The disadvantage of hydrazine hydrate and hydroquinone is that they are highly toxic and cannot meet the needs of environmental protection; sodium borohydride has low reduction efficiency due to its easy hydrolysis

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] Step 1: Dissolve 15 mL of concentrated H 2 SO 4 , 2.5g K 2 S 2 o 8 and 2.5g P 2 o 5 After mixing evenly, place in a beaker, heat to 80°C, add 5g of graphite powder into the beaker, react for 6h, wash, filter and dry.

[0027] Step 2: Add the graphite powder and sodium nitrate processed in step 1 to the concentrated 115mL H in an ice-water bath. 2 SO 4 Add potassium permanganate slowly under stirring, heat the oil bath to 35°C, react for 3 hours, then add deionized water, heat up to 98°C, keep warm for 0.5h, then dropwise add hydrogen peroxide with a mass fraction of 30% to reduce the unreacted Potassium permanganate, washed and centrifuged to obtain graphite oxide.

[0028] Step 3: Add the graphite oxide prepared in Step 2 into water, and then treat it under 300W ultrasonic power for 0.5h, centrifuge at 8000rpm for 5min, remove the precipitate, and obtain a 1mg / L graphite oxide dispersion.

[0029] Step 4: Add sodium diphenylamine sulfonate to the graphite oxid...

Embodiment 2

[0031] According to the preparation method of Example 1, only the reaction mass ratio of step 4 is changed to 30:0.407.

[0032] Figure 1 to Figure 4 The powder XRD diffraction spectrogram, the transmission electron microscope figure, the scanning electron microscope and the Raman spectrogram of the graphene that the present embodiment makes are provided respectively, find out from the powder XRD diffractogram, the (001) diffraction peak of graphite oxide is 11.28 ° , after the reduction reaction with sodium diphenylamine sulfonate, the (002) diffraction peak appeared at 23.14°; from the transmission electron microscope and scanning electron microscope, it can be seen that the graphene sheets have folds and stacked on each other; from the Raman spectrum, The D peak of graphene oxide appears at 1350 cm -1 and G peak at 1602 cm -1 , the D peak of graphene is at 1347cm -1 And the G peak is at 1598cm -1 , similar to related reports, the results show that graphene is prepared...

Embodiment 3

[0034] Press the preparation method of embodiment 1, just change the reaction mass ratio of step 4 into 30:0.542, Figure 5 It is the powder XRD diffraction spectrogram of the graphene of the present embodiment, and the results show that graphene is prepared by the method of the present invention, and the transmission electron microscope figure, scanning electron microscope and Raman spectrum figure are similar to embodiment 2.

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Abstract

The invention belongs to the field of two-dimensional nano materials and preparation thereof, and particularly relates to a preparation method of graphene. The method is characterized by comprising the following steps: adding a reducer into a graphite oxide dispersion liquid, heating to react, and carrying out centrifugal separation to obtain the graphene, wherein the reducer is sodium diphenylamine sulfonate. The method has the advantages of more sufficient reduction of graphite oxide, easy product separation and simple purification process. In the preparation process, no stabilizer or dispersant is added, and the obtained graphene contains fewer impurity elements; and the invention has the characteristics of controllable process, short period, atmospheric conditions, simple equipment and excellent graphene properties, is suitable for industrial production, and has wide application prospects in the technical fields of catalysis, energy transfer and storage, sensors and the like.

Description

technical field [0001] The invention belongs to the field of two-dimensional nanometer materials and their preparation, in particular to a preparation method of graphene. Background technique [0002] Graphene is sp 2 Single-atom-layer planar crystals formed by hybridized carbon atoms arranged in a honeycomb grid in two-dimensional space are the basic units of fullerenes, carbon nanotubes and graphite. Since Professor A. Geim of the University of Manchester and Since its first successful preparation by its collaborators, graphene, as a rapidly rising star in the field of material science and condensed matter physics, has attracted many scientists to study various aspects of it. Studies have shown that the theoretical specific surface area of ​​graphene is as high as 2630m 2 / g, the Young's modulus is 1100Gpa, the breaking strength is 125Gpa, the mechanical strength is 1060Gpa, the thermal conductivity is 5000W / m·k, and the electron mobility at room temperature is 15000cm 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 刘琦纪云洲李占峰包金婷陈林提程美令
Owner 苏州汇涵医用科技发展有限公司
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