A kind of low temperature thermoforming method of three-dimensional graphene material

A molding method and graphene technology, applied in graphene, chemical instruments and methods, structural parts, etc., can solve the problems of complex preparation methods of three-dimensional graphene materials, volume shrinkage of three-dimensional graphene, and unsuitability for large-scale production, etc., to achieve The effect of low cost, friendly environment and mild conditions

Active Publication Date: 2019-05-31
HUAZHONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above defects or improvement needs of the prior art, the present invention provides a low-temperature thermoforming method for three-dimensional graphene materials, the purpose of which is to control the reduction of graphene oxide by selecting and optimizing key reactants and their reaction conditions To achieve the preparation of three-dimensional graphene and its functional materials in a low-temperature, simple, easy-to-operate and suitable for large-scale production, thereby solving the complex preparation methods of three-dimensional graphene materials in the prior art, harsh reaction conditions, and not suitable for large-scale production. High reaction temperature leads to technical problems of three-dimensional graphene volume shrinkage and sheet stacking

Method used

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  • A kind of low temperature thermoforming method of three-dimensional graphene material
  • A kind of low temperature thermoforming method of three-dimensional graphene material
  • A kind of low temperature thermoforming method of three-dimensional graphene material

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Embodiment 1

[0050] At first preferably adopt oxidation exfoliation method (Hummers method) to prepare graphene oxide aqueous solution, its specific process is as follows: get 5g natural flake graphite powder, it is mixed with the sodium nitrate of 115mL vitriol oil and 2.5g under ice-bath condition, then Slowly add 15.0g of potassium permanganate to the solution, stir for 2 hours, raise the temperature to 35 degrees, continue stirring for 2 hours, slowly add 230mL of deionized water, then further raise the temperature to 95 degrees, and maintain 30 Minutes, then add about 500mL of deionized water to the solution, adjust the temperature to room temperature, add 12.5mL of hydrogen peroxide solution, filter the solution to obtain a solid, and successively wash with dilute hydrochloric acid and deionized water to obtain oxidation graphene solution.

[0051] The obtained graphene oxide solution was fixed to a mass concentration of 5.0mg / mL, and 2000mL of graphene oxide solution was taken in a ...

Embodiment 2

[0054] The graphene oxide aqueous solution was prepared by the oxidation exfoliation method (Hummers method) of Example 1, and the obtained graphene oxide solution was fixed to a mass concentration of 3.0 mg / mL. Take 5mL of the solution and add 0.2mL of pyrrole monomer, mix evenly, and then pour the mixture into a petri dish. The reaction temperature of the whole system is controlled at 70°C, and the reaction time is 12 hours. After the reaction, the three-dimensional assembly film is taken out. And use deionized water to clean the surface and dialysis, the specific optical picture can be found in the attached Image 6 . Then, the film is placed in a freeze dryer for freeze-drying to obtain a three-dimensional porous graphene assembly film material, and the thickness of the film can be regulated by the volume of the injected mixed solution.

Embodiment 3

[0056] The graphene oxide aqueous solution was prepared by the oxidation exfoliation method (Hummers method) of Example 1, and the obtained graphene oxide solution was fixed to a mass concentration of 10.0 mg / mL. Take 2mL of the solution and add 0.1mL of pyrrole monomer, mix well, then inject the mixed solution into the capillary, the reaction temperature of the whole system is controlled at 75°C, and the reaction time is 2 hours. Assemble the body fiber, and wash the surface and dialyze with deionized water, the specific physical picture can be found in the attached Figure 7 . Next, the fibers are placed in a freeze dryer for freeze-drying to obtain three-dimensional porous graphene assembly fibers. The diameter of the fiber can be tuned by the diameter of the capillary.

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Abstract

The invention discloses a method for preparing a three-dimensional graphene material. The method includes the following steps that 1, a graphene oxide solution with the concentration of 1-20 mg / ml is prepared through an oxidation stripping method; 2, the graphene oxide solution prepared in the step 1 is mixed with a reductive polymerization monomer to obtain a mixed liquid, wherein the volume fraction of the reductive polymerization monomer in the mixed liquid is 0.5-5%; then the mixed liquid is reacted at 60-80 DEG C for 1-12 hours, the reaction product is cooled to the room temperature, and a three-dimensional graphene assembly body can be obtained; 3, the three-dimensional graphene assembly body obtained in the step 2 is subjected to freeze-drying to obtain the three-dimensional graphene material. Through the selection and optimization of the key reactants and reaction conditions of the key reactants, the reduction degree of graphene oxide is controlled, and the method achieves low-temperature operation and is simple and easy to operate and suitable for the large-scale production of three-dimensional graphene and its functional materials.

Description

technical field [0001] The invention belongs to the technical field of three-dimensional graphene preparation, and more specifically relates to a low-temperature thermoforming method of a three-dimensional graphene material or a functional material thereof and a product thereof. Background technique [0002] Graphene is a honeycomb-like two-dimensional lattice structure carbon nanomaterial with carbon atoms tightly packed in sp2 hybrid system. Due to its excellent electrical, mechanical and thermal properties, it is widely used in catalysis, sensing, energy storage and Flexible electronic devices and other fields. The three-dimensional assembly of two-dimensional graphene sheets can realize the embedding of nanomaterials into macroscopic devices, which can broaden the application range of graphene. However, one of the main problems in the research and application of three-dimensional graphene is that graphene sheets are easy to aggregate with each other, resulting in a decr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19C01B32/194C01B32/198H01G11/30H01G11/34H01G11/36H01G11/48H01G11/24H01M4/36H01M4/587H01M4/60H01M4/96
CPCC01B2204/22C01P2002/70C01P2002/82C01P2004/01C01P2004/03C01P2004/04H01G11/24H01G11/30H01G11/34H01G11/36H01G11/48H01M4/366H01M4/587H01M4/602H01M4/96Y02E60/10Y02E60/50
Inventor 王帅张哲野徐沛
Owner HUAZHONG UNIV OF SCI & TECH
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