Preparation method of graphene

A graphene and graphite technology, applied in the field of nanomaterials, can solve the problems of large amount of reducing agent, long reaction period and incomplete reduction, and achieve the effects of less amount of reducing agent, short reaction period and easy separation.

Inactive Publication Date: 2012-01-18
HENAN UNIVERSITY
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  • Abstract
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  • Claims
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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of graphene, to overcome the technical defects of the current method such as long reaction cycle, large amount of reducing agent and incomplete reduction, and effectively solve the problem of graphene agglomeration in the reduction reflux process

Method used

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preparation example Construction

[0026] Preparation of graphite oxide:

[0027] Weigh 5g of graphite powder and 2.5g of sodium nitrate and add them to 115mL of concentrated sulfuric acid (mass concentration 98%) in an ice-water bath, add 15g of potassium permanganate while stirring, and stir the mixture for 0.5h under ice-water bath conditions; Slowly raise the temperature to 35°C for 3h, then add 15g of potassium permanganate, heat up to 45°C for 12h; add 800mL of deionized water, stir at 20°C for 1h, then dropwise add 30mL of 30% (mass concentration) peroxide Hydrogen, stir for 0.5h; filter the above solution, wash with 500mL 10% (mass concentration) hydrochloric acid solution to remove metal ions, and then wash with a large amount of deionized water to remove excess acid and wash until neutral.

[0028] Drying: vacuum-dry the above-mentioned filtered product at 70° C. for 24 hours to obtain graphite oxide.

Embodiment 1

[0030] Weigh 2g of dry graphite oxide and place it in a quartz tube, evacuate until the degree of vacuum reaches 0.1MPa, raise the temperature to 300°C at a heating rate of 50°C / min, and expand the graphite oxide to obtain exfoliated graphite oxide.

[0031] Dissolve 1 g of sodium metal in 100 mL of liquid ammonia to obtain an alkali metal / liquid ammonia solution with a concentration of 10 mg / mL, add 1 g of the above-mentioned thermally expanded and exfoliated graphite oxide to it, and stir for 0.5 h; add 50 mL of ethanol and stir for 0.5 h, Suction filtration, washing with 100 mL of diethyl ether, and finally washing with 200 mL of deionized water, and vacuum drying at 70°C for 24 hours to obtain graphene powder.

Embodiment 2

[0033] Weigh 2g of dry graphite oxide and place it in a quartz tube, evacuate until the degree of vacuum reaches 0.1MPa, raise the temperature to 500°C at a heating rate of 100°C / min, and expand the graphite oxide to obtain exfoliated graphite oxide.

[0034] Dissolve 3g of metallic calcium in 100mL of liquid ammonia to obtain an alkaline earth metal / liquid ammonia solution with a concentration of 30mg / mL, add 1g of thermally expanded and exfoliated graphite oxide to it, and stir for 2h. Add 100mL of methanol and stir for 0.5h, filter with suction, wash with 200mL of ether, and finally wash with 200mL of deionized water, and dry in vacuum at 60°C for 24h to obtain graphene powder.

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Abstract

The invention belongs to the technical field of nano-materials, and particularly relates to a preparation method of graphene. Graphite oxide is added into a liquid ammonia solution with dissolved reductive metal for reaction, and graphene is obtained after subsequent separation. The method provides more fully reduction of graphite oxide; the product is easy to separate, and the purification process is simple; in the preparation process, no stabilizer or dispersant is added, and the prepared graphene contains less impurity elements; the using amount of the reducing agent is few, and the process is controllable; the low-temperature reduction condition prevents the easy generation of the agglomeration phenomenon; the reaction period is short; a normal pressure condition is required; and the equipment is simple. The prepared graphene has wide application prospects in the electrochemistry field.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, in particular to a method for preparing graphene. Background technique [0002] Graphene is SP 2 Hybridized carbon atoms are arranged in a honeycomb-like hexagonal planar crystal with a thickness of only a single layer of atoms. It is a new type of carbon nanomaterial and is the basic unit of graphite, carbon nanotubes and fullerenes. It has novel physical and chemical properties. Studies have shown that the specific surface area of ​​graphene can be as high as 2600m 2 / g, the Young's modulus is about 1100Gpa, the breaking strength is 125Gpa, the mechanical strength is 1060Gpa, and the thermal conductivity is 5000W / m·K. Graphene also has excellent electron transport capabilities, and its electron mobility is as high as 15000 cm at room temperature. 2 / V·S. Since graphene was first discovered in 2004 (Novoselov, K.S. et al Science, 2004, 306, 606), it has immediately aroused great intere...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00
Inventor 张治军张经纬赵闯冯俊吴志申
Owner HENAN UNIVERSITY
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