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Preparation method for graphene

A technology of graphene and graphite, which is applied in the field of graphene solution phase preparation, can solve problems such as difficulty in obtaining high-quality and high-purity products, difficulty in large-scale preparation, multiple defects and impurities in graphene, and easy large-scale production , high yield, and less structural defects

Active Publication Date: 2012-05-16
NINGBO MORSH TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the first three methods can obtain high-quality graphene, it is obviously difficult to achieve large-scale preparation
The solution-phase redox preparation method is easy to expand and prepare in large quantities, but the graphene products after the redox process have many defects and impurities, and it is difficult to obtain high-quality and high-purity products
[0004] Recently, some scientists reported that the direct exfoliation of graphite was achieved by using superacid chlorosulfonic acid, and a graphene sol with a concentration of 2 mg / ml was obtained (N.Behabtu, et al., Nature Nanotechnology 2010, 5, 406), but chlorosulfonic acid Acid is extremely unstable in air and prone to explosion, so it must be operated under the protection of inert gas, which limits the scale-up of its preparation

Method used

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Experimental program
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Embodiment 1

[0025] In the first step, the above four raw materials were uniformly mixed at 30° C. and mechanically stirred for 1.5 hours according to the mass ratio of graphite: potassium permanganate: acetic anhydride: concentrated nitric acid of 1:0.4:1.7:0.5. Add water to dilute, and add 30wt.% hydrogen peroxide until no bubbles are produced. The product was washed with water until neutral and dried.

[0026] In the second step, the product in the first step was left to stand in air at 900° C. for 30 seconds, and then cooled to room temperature.

[0027] In the third step, the product in the second step was placed in air at 500° C. for 2 hours.

[0028] In the fourth step, the product obtained in the third step is dispersed in N-methylpyrrolidone solvent according to 1% by mass, and ultrasonically treated for 15 minutes to obtain a graphene suspension. After centrifugation or filtration and drying, the graphene powder material can be obtained.

[0029] Such as figure 1 As shown, th...

Embodiment 2

[0031] In the first step, the above-mentioned three raw materials were uniformly mixed at 40° C. and mechanically stirred for 1.5 hours according to the mass ratio of graphite:concentrated sulfuric acid:hydrogen peroxide of 1:5:0.2. The product was washed with water until neutral and dried.

[0032] Subsequent steps are the same as in Example 1.

Embodiment 3

[0034] In the first step, the above four raw materials were uniformly mixed at 30° C. and mechanically stirred for 1.5 hours according to the mass ratio of graphite:concentrated sulfuric acid:concentrated nitric acid of 1:5:0.2. The product was washed with water until neutral and dried.

[0035] Subsequent steps are the same as in Example 1.

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Abstract

The invention relates to a preparation method for graphene. The preparation method is characterized in that: the method comprises the following steps: 1, placing graphite in a mixed solution comprising an oxidant and an intercalation agent, and carrying out treatments of impregnation, mechanical stirring or ultrasound to obtain a primary intercalation compound; 2, carrying out a treatment for the primary intercalation compound in the air, wherein the intercalation agent is rapidly decomposed, the primary separation of the graphite intercalation compound is achieved to obtain a primary stripping material; 3, adopting a secondary intercalation method or a mild oxidation method to treat the primary stripping material to obtain a secondary intercalation compound; 4, carrying out a treatment for the second intercalation compound in the air; 5, adopting a liquid phase ultrasonic treatment, solid mechanical grinding and ball milling to achieve the complete stripping of the graphite to obtain the graphene product. Compared to the prior art, the method of the present invention has the following advantages that: the prepared graphene has characteristics of less structural defects, good conductivity and high yield; the preparation process has characteristics of simple operation and low cost, and is applicable for the large-scale production.

Description

technical field [0001] The invention relates to a solution-phase preparation method of graphene. Background technique [0002] Since its first discovery in 2004, graphene (i.e., single-layer graphite) has immediately aroused great interest in the scientific community and has become one of the hottest materials in recent years. Graphene has a very high electron transport rate due to its unique two-dimensional crystal structure, and is the material with the highest mechanical strength known. At the same time, it has stable chemical properties, transparency, and excellent thermal conductivity, so it is extremely useful in many fields. Attractive application prospects. Basic and applied research on graphene has also been in full swing worldwide. [0003] The preparation of graphene has always been a hot topic of concern, because it is directly related to the subsequent application of the material. The preparation methods that have been reported so far mainly include mechanica...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184
Inventor 刘兆平周旭峰秦志鸿
Owner NINGBO MORSH TECH
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