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Macro-preparation for big size graphene

A graphene, large-scale technology, applied in the field of graphene preparation, can solve the problems of uneven size of graphene, small size of graphene, many graphene defects, etc., and achieve uniform product size, large product size, and technological process. simple effect

Active Publication Date: 2011-04-20
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the participation of the strong oxidation process, the prepared graphene has many defects and poor quality, and the size of graphene is small (most of the sheet diameters are on the order of microns)
Recently, through the joint efforts of scientists from various countries, many improvements have been made to this method to increase the size of graphene. At present, the largest graphene size that can be obtained by this method is about 20 μm × 40 μm, but the size of graphene is not uniform. still contains a large amount of graphene with a size smaller than 10 microns

Method used

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  • Macro-preparation for big size graphene
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  • Macro-preparation for big size graphene

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The modified Hummers method ["Hummers method", please refer to the literature: Hummers W, Offman R Journal of The American Chemical Society 1958, 80:1339.] is used to weakly oxidize graphite: In this example, the lateral grain size of 2g is first Natural flake graphite with a thickness of about 500μm and a thickness of about 1μm~500μm is added to 2g NaNO 3 , 12g KMnO 4 With 96ml H 2 SO 4 In the mixed solution, stir for 2h at 0℃, then adjust the temperature to 35℃ and stir for 1h, and finally add 200ml distilled water and 10ml H 2 O 2 , The mixture is washed with water to neutral, thereby preparing graphite oxide.

[0027] The graphite oxide is dispersed in water, and the graphite oxide is gently exfoliated by weak ultrasound to obtain graphene oxide. Among them, the ultrasonic power is 350W, and the ultrasonic time is 10min.

[0028] Centrifuge the ultrasonically dispersed graphene oxide. First, remove the graphite oxide that has not been completely peeled off. The centrifug...

Embodiment 2

[0032] The modified Hummers method is used to weakly oxidize graphite: In this embodiment, first, 2g of natural flake graphite with a lateral grain size of about 500μm and a thickness of about 1μm~500μm is added to 2g NaNO 3 , 12g KMnO 4 With 96ml H 2 SO 4 In the mixed solution, stir at 0°C for 2h, and then adjust the temperature to 90°C (during this process, slowly add 80ml of distilled water to prevent uneven interlayer expansion of graphite caused by partial heating of the mixture, which will affect the final result Graphene oxide size), stir for 1h, and finally add 200ml distilled water and 10ml H 2 O 2 , The mixture is washed with water to neutral, thereby preparing graphite oxide.

[0033] The graphite oxide is dispersed in water, and the graphite oxide is gently exfoliated by weak ultrasound to obtain graphene oxide. Among them, the ultrasonic power is 350W, and the ultrasonic time is 10min.

[0034] Centrifuge the ultrasonically dispersed graphene oxide. First, remove the g...

Embodiment 3

[0037] The modified Hummers method is used to weakly oxidize graphite: In this embodiment, first, 2g of natural flake graphite with a lateral grain size of about 500μm and a thickness of about 1μm~500μm is added to 2g NaNO 3 , 24g KMnO 4 With 96ml H 2 SO 4 In the mixed solution, stir for 2h at 0℃, then adjust the temperature to 35℃, stir for 2h, and then adjust the temperature to 90℃ (during this process, slowly add 80ml of distilled water dropwise to prevent local heating of the mixture causing graphite Uniform interlayer expansion, thus affecting the size of the final graphene oxide), stir for 1h, and finally add 200ml distilled water and 10ml H 2 O 2 , The mixture is washed with water to neutral, thereby preparing graphite oxide.

[0038] The graphite oxide is dispersed in water, and the graphite oxide is gently exfoliated by weak ultrasound to obtain graphene oxide. Among them, the ultrasonic power is 600W, and the ultrasonic time is 1h.

[0039] Centrifuge the ultrasonically d...

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Abstract

The invention relates to the preparation technology of graphene, in particular to a preparation method of big size graphene, which is suitable for macro-preparation of the big size graphene. The method comprises the following steps of: (1) with a big size graphite as a raw material, carrying out weak oxidation on a graphite raw material by utilizing a modified Hummers method; (2) carrying out mild peeling on a graphite oxide dispersed in water by utilizing a weak ultrasonic or oscillating method to obtain the graphene oxide; (3) separating the graphene oxide through controlling a centrifugal rotation speed and a centrifugal time by utilizing a multi-centrifuging method to obtain the uniform big size graphene oxide; and (4) depositing the graphene oxide on a substrate, and reducing by utilizing hydrazine or hydrazine hydrate to obtain the high quality big size graphene. The big size graphene can be obtained in a macro amount by utilizing the method, the maximum area can reach 3*104 microns<2>, and the method lays the foundation for application of the graphene in the field of flexible photoelectric functional films, such as transparent conducting films, display and solar battery electrodes, gas sensors, optical-electrical converters, film electronic devices, and the like.

Description

Technical field: [0001] The invention relates to a preparation technology of graphene, in particular to a preparation method of large-size graphene, which is suitable for the large-scale preparation of large-size graphene. Background technique: [0002] Graphene refers to a single layer of carbon atoms densely packed into a two-dimensional honeycomb lattice structure. It is the basic structural unit for building other dimensional carbon materials (zero-dimensional fullerenes, one-dimensional carbon nanotubes, and three-dimensional graphite). Due to its excellent electrical, thermal and mechanical properties, graphene is expected to be widely used in high-functional nanoelectronic devices, transparent conductive films, composite materials, catalytic materials, energy storage materials, field emission materials, gas sensors, and gas storage. Therefore, since the research group of the University of Manchester in the United Kingdom obtained stable graphene for the first time in 2004,...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 成会明任文才赵金平裴嵩峰高力波吴忠帅
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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