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Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling

A chemical method and layer peeling technology, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve problems such as high oxygen content, high energy consumption in the electrode process, complex process, etc., and achieve high conductivity and time-consuming The effect of short, simple preparation method

Inactive Publication Date: 2016-09-21
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing graphene by intercalation and exfoliation of graphite by liquid phase chemical method in order to solve the problems of complex process, high energy consumption in the electrode process and high oxygen content in the existing graphene preparation method

Method used

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  • Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling
  • Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling
  • Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling

Examples

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Embodiment 1

[0034] Add 10g of expanded graphite (25 mesh) to 200mL of mixed acid (concentrated sulfuric acid and concentrated nitric acid), and then add perchloric acid, where concentrated H 2 SO 4 / HClO 4 / Concentrated HNO 3 =0.5 / 1 / 1. Stir and seal well. After 30 minutes of ultrasonic treatment, magnetically stir for 6 hours, then slowly add 100 mL of hydrazine hydrate solution to the mixture while stirring, and stir for 2 minutes. The above mixture will expand rapidly. It becomes a black viscous colloid, the gel is washed with deionized water to neutrality, and the super-swelling treatment is 30 min to obtain an aqueous dispersion of graphene.

[0035] figure 1 These are scanning electron micrographs (a) and transmission electron micrographs (b) of graphene prepared in Example 1 of the present invention; figure 1 In a, it can be seen that the graphite has been peeled off by the mixed acid intercalation and the violent reaction with the reducing agent. Due to the very violent reaction, many f...

Embodiment 2

[0039] Add 10g of flake graphite (200 mesh) to 1L of mixed acid (concentrated sulfuric acid and concentrated nitric acid), then add bromic acid, of which concentrated H 2 SO 4 / HBrO 3 / Concentrated HNO 3 =8 / 1 / 3, stir evenly and seal well. After 30 minutes of ultrasonic treatment, magnetically stir for 24 hours, then slowly add 500mL hydrazine hydrate solution to the mixture while stirring, and stir for 10 minutes. The volume of the above mixture will expand rapidly. It becomes a black viscous colloid, the gel is washed with deionized water to neutrality, and the super-swelling treatment is 30 min to obtain an aqueous dispersion of graphene.

[0040] The experimental results show that the oxygen content of the graphene prepared in Example 2 is 1.98%.

Embodiment 3

[0042] Add 10g flake graphite (100 mesh) to 500mL mixed acid (concentrated sulfuric acid and concentrated nitric acid), and then add periodic acid, which contains concentrated H 2 SO 4 / HIO 4 / Concentrated HNO 3 =3 / 1 / 2. Stir and seal well. After ultrasonic treatment for 30 minutes, magnetically stir for 12 hours, then slowly add 300mL hydrazine hydrate solution to the mixture while stirring, and stir for 5 minutes. The volume of the above mixture will expand rapidly. It becomes a black viscous colloid, the gel is washed with deionized water to neutrality, and the super-swelling treatment is 30 min to obtain an aqueous dispersion of graphene.

[0043] The experimental results show that the oxygen content of the graphene prepared in Example 3 is 1.71%.

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Abstract

The invention provides a method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling, and belongs to the technical field of graphene materials. The problems of complex technology, large energy consumption in the electrolysis process and high oxygen content of present graphene preparation methods are solved. The method comprises the following steps: immersing graphite in a mixed acid solution, adding an intercalator, stirring graphite, the mixed acid solution and the intercalator to obtain a mixed solution; and adding an organic reagent to the mixed solution, and reacting to obtain a water dispersion of graphene. A special reagent is used to carry out intercalation treatment, and a sharp chemical reaction is carried out to instantly gasify the reagent between graphite layers in order to peel graphite into graphene. The yield of graphene prepared through the method is extremely high, the weight of the obtained graphene is almost same to the weight of graphite, the graphene has extremely few defects, the oxygen content of the prepared graphene is 1.63% and is extremely low, and the conductivity of the graphene is high.

Description

Technical field [0001] The invention belongs to the technical field of graphene materials, and specifically relates to a method for preparing graphene by intercalating and exfoliating graphite by a liquid phase chemical method. Background technique [0002] Since the advent of graphene in 2004, it has received extensive scientific attention due to its extremely excellent electrical properties. For example, its carrier transport behavior is similar to that of neutrinos in the theory of relativity, and the quantum Hall effect and bipolar field effect can be observed at room temperature. In addition, the unique physical and mechanical properties of graphene have further broadened its application space: extremely high Young's coefficient, thermal conductivity as high as 5300W / mK, and theoretical specific surface area as high as 2630m 2 / g, and the energy gap is adjustable, almost completely transparent, only absorbing 2.3% of light, and other excellent properties. In the near future...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B2204/04C01B2204/32C01P2002/72C01P2002/82C01P2004/03C01P2004/04
Inventor 牛利吴同舜
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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