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A method for preparing ultra-dispersed graphene by liquid nitrogen quenching

A graphene and hyper-dispersion technology, applied in the field of macro-scale preparation of hyper-dispersed graphene, can solve the problems of increasing the graphene preparation period and affecting the quality of the prepared graphene, and achieves the effects of short preparation period, shortened period and simple process

Active Publication Date: 2016-05-25
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has defects. Since the surfactant is added in this process, the surface activity needs to be removed in the subsequent preparation process, which undoubtedly increases the preparation cycle of graphene, and if the surfactant does not Complete removal will affect the quality of prepared graphene

Method used

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  • A method for preparing ultra-dispersed graphene by liquid nitrogen quenching
  • A method for preparing ultra-dispersed graphene by liquid nitrogen quenching

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Use 32 mesh natural flake graphite to prepare graphite oxide by modified Hummers method. Graphite flakes are prepared under the conditions of oxidation temperature of 35°C and oxidation time of 2h. The graphite oxide is dispersed in water, ultrasonic time is 10min, ultrasonic power is 600W, and then visible particles are removed by centrifugal speed 3000rpm to obtain graphite oxide Olefin solution.

[0022] The graphene oxide solution with a concentration of 0.5 mg / ml was heated to 40° C. and placed directly in liquid nitrogen for quenching until the solution was completely frozen, and then it was freeze-dried in situ. After drying, the hyperdispersed graphene oxide material is obtained, which is then reduced at 900°C under the protection of Ar gas, thereby obtaining hyperdispersed graphene.

[0023] Electron microscope observation results show that: under this condition, more than 90% of the graphene flakes in the graphene powder are in a small-layer dispersion state. Suc...

Embodiment 2

[0025] The preparation method of the graphene oxide solution is the same as in Example 1.

[0026] The graphene oxide solution with a concentration of 2mg / ml was heated to 40°C and directly placed in liquid nitrogen for quenching until the solution was completely frozen, and then it was freeze-dried in situ. After drying, the hyperdispersed graphene oxide material is obtained, which is then reduced at 900°C under the protection of Ar gas, thereby obtaining hyperdispersed graphene.

[0027] Electron microscope observation results show that: under this condition, more than 85% of the graphene flakes in the graphene powder are in a small-layer dispersion state.

Embodiment 3

[0029] The preparation method of the graphene oxide solution is the same as in Example 1.

[0030] The graphene oxide solution with a concentration of 6mg / ml was heated to 40°C and directly placed in liquid nitrogen for quenching until the solution was completely frozen, and then it was freeze-dried in situ. After drying, the hyperdispersed graphene oxide material is obtained, which is then reduced at 900°C under the protection of Ar gas, thereby obtaining hyperdispersed graphene.

[0031] Electron microscope observation results show that: under this condition, more than 80% of the graphene flakes in the graphene powder are in a small-layer dispersion state. Such as figure 2 As shown, the 6mg / ml graphene oxide solution was directly put into liquid nitrogen after being heated to 40°C to be chilled. It can be seen from the photographs of the scanning electron microscope that the high-concentration graphene oxide solution was quenched and the graphene sheets It can also maintain a ...

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Abstract

The invention discloses a method for preparing ultra-dispersed graphene by liquid nitrogen quenching. The invention adopts a chemical method to prepare graphene oxides of different sizes, heats a graphene oxide solution and then quenches it in liquid nitrogen to prepare super-dispersed graphene oxide. Then, the ultra-dispersed graphene oxide is reduced by heating or chemical reduction to prepare the ultra-dispersed graphene. The method has the advantages of low cost, simple process, and can shorten the preparation cycle (mainly shorten the cycle of sample freeze-drying), and is suitable for macro-preparation of ultra-dispersed graphene.

Description

technical field [0001] The invention relates to a graphene preparation technology, in particular to a method for preparing ultra-dispersed graphene by cooling a graphene oxide solution under a liquid nitrogen environment, and is suitable for macro-preparation of ultra-dispersed graphene. Background technique [0002] Graphene is a new type of nano-carbon material that is the most popular research at present. This material has many excellent properties, such as: peculiar quantum Hall effect, high Young's modulus (~1,100GPa), high elastic modulus (130GPa ), good thermal conductivity (~5,000Wm -1 K -1 ), high electron mobility (200,000cm 2 V -1 the s -1 ), high specific surface area (theoretical calculation value, 2,630m 2 g -1 ), good light transmission, easy to functionalize, etc. These excellent properties also make graphene have broad application prospects in many fields such as nanoelectronic devices, transparent conductive films, electrode materials, and composite ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 阎兴斌赵金平薛群基
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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