Preparation method of flawless graphene

A graphene, defect-free technology, applied in the field of preparation of defect-free graphene, can solve the problems affecting the mechanical properties, electrical conductivity and thermal properties of graphene, reduce the theoretical performance of graphene, reduce the performance of samples, etc., and achieve low production cost , Complete lattice structure and small size effect

Active Publication Date: 2018-10-02
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AI-Extracted Technical Summary

Problems solved by technology

However, the existence of structural defects greatly reduces the theoretical properties of graphene, affecting the mechanical, conductive, and thermal properties of graphene.
At present, the methods of exfoliating graphene mainly include liquid phase ex...
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The invention belongs to the field of graphene preparation and discloses a preparation method of flawless graphene. The preparation method includes the steps of S1, dispersing graphite powder into a mixed solvent formed by ethanol and 30wt% hydrogen peroxide according to the volume ratio of (1-9):(1-9), adding polyvinyl pyrrolidone, and performing ultrasonic treatment for 2-3 hours; S2, placing the solution obtained after the ultrasonic treatment in S1 into a supercritical reaction kettle, performing reaction at 40-80 DEG C and 12-20MPa for 1-3 hours, taking out the reaction solution after thereaction, and performing ultrasonic treatment on the reaction solution for 2-3 hours; S3, performing first centrifugal separation on the solution obtained after the ultrasonic treatment in S2 at 6000-8000rpm, taking the upper solution, performing second centrifugal separation on the upper solution at 15000-20000rpm, and using ethanol to centrifugally wash the product; S4, drying the product obtained in S3 to obtain the flawless graphene. The preparation method has the advantages that the graphene prepared by the method is small in size and few in layers as compared graphene prepared by otherpreparation methods, and more importantly, the graphene is complete in lattice structure and is almost flawless.

Application Domain

Single layer grapheneBulk chemical production

Technology Topic

SolventCvd graphene +6


  • Preparation method of flawless graphene
  • Preparation method of flawless graphene
  • Preparation method of flawless graphene


  • Experimental program(3)
  • Comparison scheme(3)

Example Embodiment

[0024] Example 1
[0025] S1. Disperse 50 mg of graphite powder (original graphite powder without any pretreatment and/or modification) in 10 mL of ethanol (analytical grade) and 30wt% hydrogen peroxide in a volume ratio of 2:8 In the mixed solvent, 200 mg of the surfactant polyvinylpyrrolidone was dissolved in the above mixed solution and treated with ultrasound for 3 h;
[0026] S2. Place the solution obtained after S1 sonication in a supercritical reactor, and set the reaction temperature and pressure to 40 ℃ and 20 MPa respectively. After reacting for 3 hours, take out the reaction solution and perform ultrasonic treatment on it for 3 hours;
[0027] S3. The solution obtained after S2 sonication was first centrifuged at 6000 rpm for 40 minutes, and the upper layer solution was taken and then centrifuged at 20000 rpm for the second time for 20 minutes. The product was washed with ethanol (analytical grade) and 20,000 rpm. Centrifuge for 30 minutes, and repeat the process of ethanol washing and centrifugal separation 3 times;
[0028] S4. Dry the product obtained from S4 at a temperature of 60°C to obtain a graphene sample.
[0029] See the atomic force microscope photo of the obtained graphene sample figure 1. by figure 1 It can be seen that the prepared graphene is single-layer or few-layer nanosheets.
[0030] See the TEM picture of the obtained graphene sample figure 2. by figure 2 It can be seen that the prepared graphene has a single-layer or few-layer structure, and the lateral size ranges from tens of nanometers to hundreds of nanometers.
[0031] The Raman spectrum of the raw graphite powder and the obtained graphene sample can be seen image 3. by image 3 It can be seen that compared with the raw graphite powder, the graphene sample prepared by the present invention does not have a density peak in the D zone, and it is known from the literature that the D zone peak represents the degree of lattice defects of the graphene. At this stage, the D zone The peak intensity is almost 0, indicating that the graphene lattice structure prepared by this method is complete and defect-free.
[0032] The XRD patterns of the raw graphite powder and the prepared graphene are shown in Figure 4. by Figure 4 It can be seen that the XRD diffraction peak of the graphene sample prepared by the present invention corresponds well to the diffraction peak of the raw graphite powder, indicating that the prepared graphene lattice structure is complete.

Example Embodiment

[0033] Example 2
[0034] The difference from Example 1 is that in S2, the reaction pressure is changed to 12, 14, 16 and 18 MPa; the others are the same as in Example 1.

Example Embodiment

[0035] Example 3
[0036] The difference from Example 1 is that in S2, the reaction temperature is changed to 60 and 80°C; the others are the same as in Example 1.


no PUM

Description & Claims & Application Information

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