Method for preparing and purifying graphene by microwave radiation under vacuum

A technology of microwave radiation and graphene, applied in the field of material preparation and purification, to achieve high production efficiency, low production cost, and low microwave radiation power

Inactive Publication Date: 2011-01-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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Examples

Experimental program
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Example Embodiment

[0010] Example 1

[0011] 2g of graphite powder and 1g of sodium nitrate were uniformly mixed with 46mL of sulfuric acid with a mass concentration of 98%, stirred in an ice-water bath, slowly added 6g of potassium permanganate, reacted for 2h, and then transferred to a constant temperature water bath at 35°C for 30min. After adding 92 mL of deionized water dropwise, the temperature was raised to 98 °C and the reaction was continued for 3 h, taken out from the water bath, further diluted with deionized water, and treated with 20 mL of 30% hydrogen peroxide solution to reduce the oxidizing substances in the solution. . The impurities in the dissolved solution were washed with 5% hydrochloric acid, centrifuged while hot, and the filter cake was repeatedly washed with deionized water until the pH value of the washing solution was greater than 5, and vacuum dried at 70°C for 48 hours to obtain graphite oxide.

[0012] Take 2 g of the graphite oxide obtained in the previous step an...

Example Embodiment

[0013] Example 2

[0014] The process and conditions of this example are the same as those of Example 1, except that the power of the microwave is adjusted to 1500W, and the irradiation time is adjusted to 100s, and the graphene sample can still be obtained. The samples were tested by XPS and specific nitrogen surface area tester. The test results showed that the atomic ratio of oxygen in graphene was about 7%, and the specific surface area was about 500m. 2 / g.

Example Embodiment

[0015] Example 3

[0016] According to the preparation method of Example 1, the power of the microwave is adjusted to 2000W, the radiation time is adjusted to 2s, and other reaction conditions remain unchanged, and the graphene sample can be obtained.

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Abstract

The invention discloses a method for preparing and purifying graphene by microwave radiation under vacuum. The method for preparing graphene is as follows: placing graphite oxide in a reactor, radiating the graphite oxide by microwaves under vacuum, and obtaining the graphene by heating and cleavage of the graphite oxide. The method for purifying graphene is as follows: placing graphene with low purity in a reactor, irradiating the graphite oxide by microwaves under vacuum, and obtaining the graphene with higher purity after impure graphene is subjected to heating and cleavage. The method is implemented under the vacuum condition, thus being favor to preventing the generated graphene from being oxidized by oxygen in the reactor, reducing the cleavage resistance of the graphite oxide, and ensuring the safety in the operation process, and the method also has the advantages of high production efficiency, low production cost, safe operation process, high product purity and the like, and can be used as one of the methods for preparing and purifying graphene massively.

Description

technical field [0001] The invention relates to a method for preparing and purifying graphene by microwave radiation under vacuum, which belongs to the preparation and purification technology of materials. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered in 2004, which is a single-layer or multi-layer extremely thin carbon material. Since the day it was discovered, it has become one of the research hotspots in the fields of carbon materials, nanotechnology, condensed matter physics and functional materials. [0003] At present, the main preparation methods of graphene are mechanical splitting method, epitaxial crystal growth method, chemical vapor deposition method, chemical cleavage and reduction method of graphite oxide. Other preparation methods have also been developed, such as gas phase plasma growth technology, electrostatic deposition method and high temperature and high pressure synthesis method. Yang Quanhong et al. used t...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 杨全红魏伟苏方远陈学成吕伟
Owner TIANJIN UNIV
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