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
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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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