Preparation method of graphene

A technology of graphene and graphite, which is applied in the field of material preparation, can solve the problems of high oxygen content of graphene, easy explosion, limited application, etc., and achieve the effect of simple operation and high degree of reduction

Inactive Publication Date: 2014-09-10
NANCHANG UNIV
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Problems solved by technology

Although the reduction time of this method is short, the hydrogen concentration is high, it is prone to explosion, and the safety is not good, and the generated graphene has a high oxygen content and a C / O ratio of 4.
Ching-Yuan Su et al. reported in ACS NANO, 4(9), 5286, 2010, that graphene oxide was deposited on a silicon dioxide substrate to form a single-layer graphene oxide film, and then in argon-hydrogen mixed gas (hydrogen volume Concentration is 20 %) heated to 900 ℃ reduction exfoliation to obtain graphene, but this method has a small amount of graphene and is difficult to separate from the substrate, which limits its application and is difficult to scale production

Method used

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Examples

Experimental program
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Embodiment 1

[0019] Technical route: (1) graphite → (2) preparation of graphite oxide → (3) crushing of graphite oxide → (4) reduction of graphite oxide to graphene.

[0020] (1) Graphite: 99.9% purity

[0021] (2) Graphite oxide: Weigh 12 g of graphite with a purity of 99.9% in (1), add 10 g of potassium peroxodisulfate (analytical pure), 10 g of phosphorus pentoxide (analytical pure), 48 mL of concentrated sulfuric acid (mass Fraction 98%) in a round-bottomed flask, stirred and reacted in a water bath at 80 °C for 4.5 h, after the reaction was completed, 500 mL of deionized water was added, filtered and washed until neutral, and dried at 60 °C to obtain pre-oxidized graphite. Weigh 2 g of the above-mentioned pre-oxidized graphite, add 1 g of sodium nitrate (analytical pure), 46 mL of concentrated sulfuric acid, stir in ice bath for 30 min, slowly add 6 g of potassium permanganate (analytical pure), and react for 45 min in ice bath. min. Then the mixture was heated to 35 °C, stirred for...

Embodiment 2

[0026] The same method as in Example 1 was used to prepare small pieces of graphite oxide, and the small pieces of graphite oxide were placed in a nitrogen-hydrogen mixed flow, the hydrogen volume concentration was 5%, the flow rate was 40 mL / min, and the mixture was raised to 300 ℃, kept for 15 min, and finally cooled down to room temperature in nitrogen-hydrogen mixed gas (flow rate 40 mL / min) to obtain graphene with a specific surface area of ​​285 m 2 / g.

Embodiment 3

[0028] The same method as in Example 1 was used to prepare small pieces of graphite oxide, and the small pieces of graphite oxide were placed in the nitrogen-hydrogen mixed flow, the hydrogen volume concentration was 5%, the flow rate was 60 mL / min, and the mixture was raised to Keep at 400 ℃ for 2 h, and finally cool down to room temperature in nitrogen-hydrogen mixed gas (flow rate 60 mL / min) to obtain graphene with a specific surface area of ​​326 m 2 / g.

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Abstract

The invention discloses a preparation method of graphene, which comprises the following steps: (1) breaking graphite oxide into small pieces by a mechanical shearing or ball milling way; and (2) in a hydrogen nitrogen or hydrogen argon atmosphere, heating the small pieces of graphite oxide to 250-500 DEG C in the conditions that the volume concentration of hydrogen is 1-19%, the concentration of nitrogen or argon is 99-81%, the gas flow rate is 10-100mL/min and the heating speed is 5-35 DEG C per minute; preserving heat for 5-120min; and enabling the hydrogen nitrogen or hydrogen argon flow to drop to room temperature or naturally cooling to room temperature to obtain graphene. The invention provides a safe and low-cost method for preparing graphene through hydrogen reduction based on the reduction and stripping at low hydrogen concentration and low temperature of the small pieces of graphite oxide. The method is simple to operate, and the obtained graphene has relatively high reduction degree.

Description

technical field [0001] The invention belongs to the field of material preparation. Background technique [0002] Graphene has excellent physical properties due to its single-layer sheet-like structure composed of carbon atoms, such as high theoretical specific surface area, excellent mechanical strength, good flexibility and high electrical conductivity, etc., so it is used in many fields. Exciting application prospects. [0003] The reduction of graphene oxide is an important and low-cost route to prepare graphene. Generally, graphite oxide is first ultrasonically dispersed in water or an organic solvent for a long time to obtain a graphene oxide solution, and then the graphene oxide is reduced to a graphene solution using reducing agents such as sodium borohydride and hydrazine hydrate. Or long-term ultrasonic dispersion in organic solvents, it is difficult to be suitable for large-scale production; although the obtained graphene has a high degree of reduction, the reduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/192
Inventor 李越湘张伟英彭绍琴
Owner NANCHANG UNIV
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