Graphene and preparation method thereof

A graphene and graphite technology, applied in the field of graphene and its preparation, can solve the problems of graphene damage, incomplete lamella structure, many defects, etc., and achieve the effect of low energy consumption

Inactive Publication Date: 2015-07-22
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sheet structure of graphene prepared by the oxidation-reduction method disclosed in the pr

Method used

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  • Graphene and preparation method thereof
  • Graphene and preparation method thereof

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preparation example Construction

[0028] The invention provides a kind of preparation method of graphene, comprises the following steps:

[0029] a), carry out first reaction after graphite, acid and oxidizing agent are mixed, obtain graphite intercalation compound, described acid comprises concentrated sulfuric acid, and described oxidizing agent comprises chlorate;

[0030] b), performing a second reaction with the graphite intercalation compound and a peroxide to obtain an intermediate product, the peroxide comprising hydrogen peroxide;

[0031] c), performing ultrasonic stripping on the intermediate product to obtain graphene.

[0032] The present invention adopts concentrated sulfuric acid and chlorate to oxidize graphite, and the oxidation of graphite by concentrated sulfuric acid and chlorate oxidation system is relatively weak, so that the degree of destruction of the sheet structure of prepared graphene is small; In the process of preparing graphene, hydrogen peroxide will react with the concentrated...

Embodiment 1

[0056] 10g of natural graphite with a particle size of 150 μm and 200g of mass concentration are mixed evenly with 98% concentrated sulfuric acid, and then 40g of NaClO is added to the resulting mixture. 3 Carrying out the first reaction at 15° C. for 12 hours to obtain a graphite intercalation compound;

[0057] Add 60g of 30% aqueous hydrogen peroxide solution to the graphite intercalation compound and carry out the second reaction at 30°C to obtain a gray-black worm-like reaction product; filter the reaction product with filter paper and wash with water until neutral , to get the intermediate product;

[0058] Dispersing the intermediate product in water, performing ultrasonic exfoliation at 1000w for 10 min to obtain a graphene solution; freeze-drying the graphene solution to obtain a graphene powder.

[0059] The present invention carries out Raman spectrum analysis with the graphene powder that embodiment 1 obtains, and the result is as follows figure 1 as shown, figu...

Embodiment 2

[0063] 10g particle size is 500 μm expanded graphite and 400g mass concentration is the concentrated sulfuric acid of 90% and mixes evenly, then adds the NaClO of 100g in the mixture that obtains 3 Carry out the first reaction at 60 DEG C for 24 hours to obtain graphite intercalation compound;

[0064] Add 50 g of aqueous hydrogen peroxide solution with a mass concentration of 60% to the graphite intercalation compound, and perform a second reaction at 180° C. to obtain a gray-black worm-like reaction product; filter the reaction product with a filter bag and wash with acetone To neutrality, an intermediate product is obtained;

[0065] Dispersing the intermediate product in water, performing ultrasonic peeling at 1000w for 20min to obtain a graphene solution; spray drying the graphene solution in a spray machine to obtain a graphene powder.

[0066] The graphene powder obtained in embodiment 2 is analyzed and tested according to the method described in embodiment 1, and the ...

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Abstract

The present invention provides a graphene preparation method, which comprises: a), mixing graphite, an acid and an oxidizing agent, and carrying out a first reaction to obtain a graphite intercalation compound, wherein the acid comprises concentrated sulfuric acid, and the oxidizing agent comprises a chlorate; b), carrying out a second reaction of the graphite intercalation compound and a peroxide to obtain an intermediate product, wherein the peroxide comprises hydrogen peroxide; and c), carrying out ultrasound stripping on the intermediate product to obtain the graphene. According to the present invention, the graphite oxidation degree through the concentrated sulfuric acid and the chlorate is weak; the concentrated sulfuric acid and the hydrogen peroxide react to release a lot of heat and gas, such that the graphite intercalation compound swells and be peeled; and the concentrated sulfuric acid and the hydrogen peroxide react to generate a lot of OH free radicals and HSO4 free radicals, and the oxygen-containing functional group on the graphite intercalation compound sheet layer can be removed through the free radicals, such that the degree of the damage on the sheet layer structure of the graphene of the present invention is low.

Description

technical field [0001] The invention relates to the field of graphite material preparation, in particular to a graphene and a preparation method thereof. Background technique [0002] Graphene is a two-dimensional material with a single-layer sheet structure composed of carbon atoms and a thickness of only one carbon atom. Graphene has many excellent properties. For example, graphene is almost completely transparent, absorbing only 2.3% of light, and its light transmission is very good; the thermal conductivity of graphene is as high as 5000W / m K, which is higher than that of carbon nanotubes and diamonds. ; The electron mobility of graphene at room temperature exceeds 15000 cm 2 / V s, which is higher than that of carbon nanotubes and silicon crystals; the resistivity of graphene is only 10 -6 Ω·cm, lower than copper or silver, is currently the material with the smallest resistivity. People use graphene's low resistivity and fast electron migration characteristics to prep...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 周旭峰刘兆平秦志鸿
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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