Preparation method of grapheme or doped graphene or graphene complex

A graphene and composite technology, applied in the field of carbon material preparation, can solve the problems of difficulty in preparing graphene products in large quantities, small, generally only tens to hundreds of nanometers, limited specific surface area, etc., to achieve the effect of convenient batch preparation.

Active Publication Date: 2012-06-20
CHINA UNIV OF PETROLEUM (BEIJING)
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Problems solved by technology

However, the use of macro-sheets, such as glass sheets, is low in cost, but the specific surface area is limited, so it is difficult to prepare graphene products in large quantities; MgO and ZnS are used as templates or cata

Method used

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  • Preparation method of grapheme or doped graphene or graphene complex
  • Preparation method of grapheme or doped graphene or graphene complex

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preparation example Construction

[0020] The invention provides a method for preparing graphene, doped graphene or graphene composite, which uses lamellar natural compounds to prepare graphene, doped graphene or graphene by vapor phase chemical deposition method or liquid phase impregnation method. Graphene composite. The lamellar natural compound is one or a mixture of kaolin, montmorillonite, vermiculite, mica, brucite and pseudo-boehmite.

[0021] In the preparation method of graphene, doped graphene or graphene composite of the present invention, the reaction temperature of the vapor phase chemical deposition method is 300°C to 1000°C, preferably 600°C to 900°C; The deposition method uses one or more mixtures of nitrogen, argon and helium as the carrier gas; uses methane, ethane, ethylene, acetylene, propane, propylene, butane, liquefied petroleum gas and carbon monoxide One or more mixtures are used as carbon source gas, such as preferably methane or ethylene; one or more mixtures of ammonia (NH3), dibor...

Embodiment 1

[0051] Weigh 20g of vermiculite and put it into a vertical fluidized bed reactor with a diameter of 50mm. The reactor is operated under normal pressure conditions, and the temperature is raised to 900°C under 0.2L / min argon flow, and then 0.6L / min Methane flow reacted for 20 minutes, and the intermediate product was taken out after cooling to room temperature. At 60-90°C, first pickle the intermediate product with hydrochloric acid solution (50% volume concentrated hydrochloric acid+50% volume deionized water); then use hydrofluoric acid solution (50% volume hydrofluoric acid+50% volume deionized water) to pickle the intermediate product to remove the vermiculite; finally wash it to neutral with deionized water and dry it at 80° C. for 12 hours to obtain 0.5 g of the final product.

[0052] Thermogravimetric analysis (TGA-2050, air flow 20ml / min, heating rate 10 ℃ / min) shows that carbon component content 97% (mass percentage composition) in the product, Raman spectrum (see fi...

Embodiment 2

[0054] Using ethylene as the carbon source gas and vermiculite as the template, it can be prepared as image 3 The graphene product shown has flakes up to a few hundred microns in size.

[0055] The preparation process is as follows: Weigh 30g of vermiculite and put it into a vertical fluidized bed reactor with a diameter of 50mm. 0.6L / min ethylene was reacted for 30 minutes, and the intermediate product was taken out after cooling to room temperature. The vermiculite was removed by hydrochloric acid pickling and hydrofluoric acid pickling (the specific method of pickling was the same as in Example 1).

[0056] Thermogravimetric analysis (TGA-2050, air flow 20ml / min, heating rate 10°C / min) shows that the carbon component content is 95% in the product, and the Raman spectrum shows that the sample has the G peak, D peak and 2D peak. Confirm through the observation of transmission electron microscope (JEM2100, JEOL), the graphene product that obtains has the graphite layer str...

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Abstract

The invention belongs to the technical field of the preparation of carbon material and provides a preparation method of grapheme or doped graphene or graphene complex. The grapheme or doped graphene or graphene complex is prepared by using the chemical vapor deposition method or liquid-phase impregnation method by taking kaolin, montmorillonite, vermiculite, mica, brucite, pseudoboehmite and other lamellar compounds as the template agent. Due to the adoption of the method, the grapheme or doped graphene or graphene complex with the lamella size of hundreds of microns can be prepared, and the batch preparation of the grapheme materials can be realized conveniently.

Description

technical field [0001] The invention belongs to the technical field of carbon material preparation, and relates to a preparation method of batch graphene, doped graphene or graphene composite. Background technique [0002] Graphene, as a new two-dimensional carbon material, was first discovered by Novoselov et al. in 2004 (Novoselov, K.S.; Geim, A.K.; Morozov, S.V.; Jiang, D.; Zhang, Y.; Dubonos, S.V. ; Grigorieva, I.V.; Firsov, A.A. Science 2004, 306, 666-9). Graphene is the thinnest and strongest material known so far. It has excellent electrical conductivity, can withstand current densities six orders of magnitude higher than copper, has record thermal conductivity, and has high hardness and good ductility at the same time. (Geim, A.K. Science 2009, 324, 1530-4). In addition, if graphene, a typical two-dimensional planar structure material, can be tailored at will, graphene materials with different properties can be obtained. This series of excellent properties of grap...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y30/00B82Y40/00B01J23/881B01J23/882C01B32/184
Inventor 宁国庆高金森
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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