Method for preparing graphene

A technology of graphene and graphite, which is applied in the field of nanomaterials, can solve the problem of not being able to meet the large-scale demand for energy storage materials and functional composite materials, the low production efficiency of mechanical exfoliation and epitaxial growth methods, and affecting the quality and performance of graphene, such as electrical conductivity. and other issues to achieve good quality, easy large-scale production, and reduced structural defects

Active Publication Date: 2012-10-31
NINGBO MORSH TECH
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Problems solved by technology

[0004] Among the above methods, the preparation efficiency of mechanical exfoliation method and epitaxial growth method is very low, and it is difficult to meet the needs of large-scale
Although the chemical vapor deposition method can obtain large-scale continuous graphene films, it is suitable for micro-nano electronic devices or transparent conductive films, but it cannot meet the large-scale needs of energy storage materials and functional composite materials.
[0005] Compared with the above three methods, the solution-phase redox method has greatly improved the scale of preparation, but the strong redox conditions in the solution-phase redox method disclosed in the prior art make the graphene product have more defects. , which seriously affects the quality and properties of graphene such as conductivity; in addition, the solution-phase redox method in the prior art is cumbersome to operate, and there are considerable difficulties in the treatment of reaction waste liquid
In summary, the methods in the prior art are not suitable for large-scale preparation of high-quality graphene

Method used

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preparation example Construction

[0023] The invention provides a kind of preparation method of graphene, comprising:

[0024] Graphene is obtained by reacting graphite in an acid solution containing an oxidizing agent.

[0025] According to the present invention, the carbon to oxygen atomic ratio in the reacted product is greater than 5, more preferably greater than 10, more preferably greater than 14, more preferably greater than 16, and more preferably greater than 20.

[0026] According to the present invention, the acid in the acid solution is one or more combinations of nitric acid, sulfuric acid, perchloric acid, hypochlorous acid, nitrous acid, chlorosulfonic acid, acetic acid, oxalic acid, but not limited thereto. The oxidant is nitric acid, sulfuric acid, perchloric acid, hypochlorous acid, nitrous acid, chlorosulfonic acid, dichromate, perchlorate, chlorate, hypochlorite, persulfate, hydrogen peroxide, peroxide combination of one or more of them, but not limited thereto. The solvent in the acid so...

Embodiment 1

[0037] The first step, potassium dichromate is mixed with 69wt% nitric acid aqueous solution, then add graphite, graphite: nitric acid: potassium dichromate: water is 1: 20: 10: 9 according to weight ratio, reacts 1 hour then at 40 ℃ Afterwards, wash with water to neutrality and dry;

[0038] In the second step, the product obtained in the first step is incubated at 900° C. for 1 minute, and then cooled to room temperature;

[0039] In the third step, the product in the second step is ground for 5 hours in a high-energy ball mill or a sand mill;

[0040] In the fourth step, the product in the third step is dispersed in ethanol, and subjected to ultrasonic treatment for 1 hour to obtain graphene with a yield of 96%, and the carbon-to-oxygen atomic ratio of the product is 21.2.

Embodiment 2

[0042] The first step, potassium dichromate is mixed with 69wt% nitric acid aqueous solution and a certain amount of ethanol, then add graphite, graphite: concentrated nitric acid: potassium dichromate: water: ethanol is 1: 20: 10: 9 according to weight ratio : 10, then after reacting for 1 hour at 40°C, wash with water to neutrality and dry;

[0043] In the second step, the product obtained in the first step is incubated at 900° C. for 1 minute, and then cooled to room temperature;

[0044] In the third step, the product in the second step is ground for 5 hours in a high-energy ball mill or a sand mill;

[0045] In the fourth step, the product in the third step is dispersed in ethanol, and subjected to ultrasonic treatment for 1 hour to obtain graphene.

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Abstract

The invention provides a method for preparing graphene. The method includes that graphite reacts in acid solution with an oxidant to obtain the graphene. Compared with the prior art, the method has the advantages that the graphene prepared by the method is good in quality, yield is greatly increased and productivity is greatly improved as compared with a mechanical exfoliation method, an epitaxial growth method and a chemical vapor deposition method; the quality of the graphene is greatly enhanced, structural defects of the graphene are greatly reduced, and electrical conductivity of the graphene is obviously improved as compared with a solution-phase oxidation reduction method; and the preparation process is simple, conditions are mild, cost is low, and large-scale production is realized easily. In addition, the graphene prepared by the method has an extremely broad prospect in fields of lithium ion batteries, super-capacitors, functional composites, transparent conductive thin films, microelectronic devices and the like.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and in particular relates to a method for preparing graphene. Background technique [0002] Since graphene was discovered in 2004, as a new type of carbon material, it has immediately aroused great interest in the scientific community. Graphene has a unique two-dimensional nanostructure, high electron transport rate, excellent electrical conductivity, high thermal conductivity, is the material with the highest mechanical strength known, and also has the advantages of stable chemical properties and good light transmission. Graphene has extremely attractive application prospects in many fields such as semiconductor industry, energy storage materials, functional composite materials, sensors and biomedicine. Therefore, basic and applied research on graphene has become an international research hotspot. [0003] The preparation method of graphene is the key issue to realize the practical appli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00C01B32/184
Inventor 刘兆平周旭峰秦志鸿唐长林
Owner NINGBO MORSH TECH
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