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Preparation method of flexible self-supporting three-dimensional porous graphene film

A graphene membrane and three-dimensional porous technology, which is applied in the field of preparation of flexible self-supporting three-dimensional porous graphene membrane, can solve the problems of immaturity of flexible porous graphene membrane, and achieve uniform and controllable pore structure, simple preparation process and excellent pore structure. developed effect

Active Publication Date: 2018-09-14
BEIJING UNIV OF CHEM TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no mature method for the research of flexible porous graphene membranes. Flexible graphene membranes generally rely on the close stacking of two-dimensional nanosheets to form films. How to introduce them into the flexible graphene structure while maintaining flexibility and strength? Porous structures are a challenge

Method used

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  • Preparation method of flexible self-supporting three-dimensional porous graphene film
  • Preparation method of flexible self-supporting three-dimensional porous graphene film
  • Preparation method of flexible self-supporting three-dimensional porous graphene film

Examples

Experimental program
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Effect test

Embodiment 1

[0024] (1) Prepare graphene oxide into 0.5 mg / mL graphene oxide aqueous solution;

[0025] (2) Add linear PVA with a molecular weight of 5000 into deionized water, stir and dissolve at a temperature of T=60°C, and prepare a PVA solution with a concentration of 5 mg / mL;

[0026] (3) Mix 100 mL graphene oxide aqueous solution with 1 mL PVA solution, stir and sonicate to disperse the two solutions evenly;

[0027] (4) Vacuum filter the mixed solution to form a film and dry to obtain a composite film of graphene oxide and PVP;

[0028] (5) The graphene oxide and PVP composite film was heated to 400 °C under the protection of nitrogen gas, and then heat-treated at constant temperature for 8 h to obtain a flexible self-supporting three-dimensional porous graphene film.

Embodiment 2

[0030] (1) Prepare graphene oxide into 1 mg / mL graphene oxide aqueous solution;

[0031] (2) Add spherical PS with a molecular weight of 10,000 into deionized water and disperse it ultrasonically to obtain a PS solution with a concentration of 50 mg / mL;

[0032] (3) Mix 100 mL of graphene oxide aqueous solution with 2 mL of PS solution, stir and sonicate to disperse the two solutions evenly;

[0033] (4) Vacuum filter the mixed solution to form a film and dry to obtain a composite film of graphene oxide and PS (such as figure 1 , the SEM of graphene oxide and PS composite film shown in 2, figure 1 is the macroscopic topography, figure 2 for partial enlargement);

[0034] (5) The graphene oxide and PS composite film was heated to 800 °C under the protection of argon gas, and then heat-treated at constant temperature for 2 h to obtain a flexible self-supporting three-dimensional porous graphene film (such as image 3 , the SEM of the porous graphene membrane shown in 4, ...

Embodiment 3

[0036] (1) Prepare graphene oxide into 10 mg / mL graphene oxide aqueous solution;

[0037] (2) Add spherical PMMA with a molecular weight of 100,000 to deionized water and disperse it ultrasonically to obtain a PMMA solution with a concentration of 10 mg / mL;

[0038] (3) Mix 1 mL of graphene oxide aqueous solution with 10 mL of PMMA solution, stir and sonicate to disperse the two solutions evenly;

[0039] (4) vacuum filter the mixed solution to form a film, and dry to obtain a composite film of graphene oxide and PMMA;

[0040] (5) The composite membrane of graphene oxide and PMMA was heated to 500 °C under the protection of helium gas, and then heat-treated at constant temperature for 6 h to obtain a flexible self-supporting three-dimensional porous graphene membrane.

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Abstract

The invention provides a preparation method of a flexible self-supporting three-dimensional porous graphene film. The preparation method comprises the following steps: selecting a high molecular polymer with low thermal stability as a templating agent, blending with graphene oxide, performing suction filtration to form a film, and then performing high-temperature heat treatment under the protection of inert gas, wherein during the high-temperature heat treatment, the graphene oxide is reduced into graphene, and the high molecular polymer with the low thermal stability is completely decomposedto leave developed pores, so that the flexible self-supporting three-dimensional porous graphene film is obtained;and the thickness of the film can be controlled within the range of 5-100 microns, thepore size is in the range of 5-100 nm, and the specific surface area is 300-1600 m<2> / g. The shape, the size and the porosity of the prepared flexible self-supporting three-dimensional porous graphene film can be conveniently regulated and controlled through the morphology (such as linear, spherical and columnar), the molecular weight and the dosage of the high molecular polymer template. The flexible self-supporting three-dimensional porous graphene film can be applied to the fields of flexible supercapacitors, flexible batteries, microelectronics, ion adsorption, membrane separation and thelike.

Description

technical field [0001] The invention relates to a preparation method of a flexible self-supporting three-dimensional porous graphene membrane. Background technique [0002] Graphene is a new type of two-dimensional nano-carbon material with high specific surface area, electrical conductivity and strength. Graphene nanosheets can self-assemble under the action of van der Waals force to form flexible graphene membranes. This kind of flexible membrane has strong mechanical properties. This special structure and unique properties make it have broad application prospects in the fields of material science, flexible energy storage, microelectronics, and membrane separation. At present, the method for preparing graphene membranes in the laboratory is mainly to prepare graphene oxide membranes by vacuum filtration, and then use chemical reduction or thermal reduction to obtain graphene membranes. The stacking of graphene sheets leads to the fact that the actual specific surface are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/52C04B35/622C04B38/06
CPCC04B35/522C04B35/62218C04B38/067
Inventor 徐斌官亦标孙宁沈进冉周淑琴朱奇珍
Owner BEIJING UNIV OF CHEM TECH
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