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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

There are no literature or patent reports on the solution to this important problem of graphene purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Mix 2g of graphite powder and 1g of sodium nitrate with 46mL of sulfuric acid with a mass concentration of 98%, stir in an ice-water bath, slowly add 6g of potassium permanganate, react for 2h, and then transfer it to a constant temperature water bath at 35°C for 30min. After adding 92mL of deionized water dropwise, raise the temperature to 98°C and continue the reaction for 3h, take it out from the water bath, further dilute with deionized water, and treat with 20mL of 30% hydrogen peroxide solution to reduce the oxidative substances in the solution . Wash the impurities in the dissolved solution with 5% hydrochloric acid, centrifuge while hot and wash the filter cake with deionized water repeatedly until the pH value of the washing solution is greater than 5, and vacuum dry at 70°C for 48 hours to obtain graphite oxide.

[0012] Get the graphite oxide 2g that last step makes, be placed in the reactor. Use a vacuum pump to evacuate, when the vacuum reaches 2Pa, stop t...

Embodiment 2

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

Embodiment 3

[0016] According to the preparation method of Example 1, only the power of the microwave is adjusted to 2000W, the radiation time is adjusted to 2s, and other reaction conditions remain unchanged, a 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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