Preparation method of three-dimensional graphene

A technology of graphene and graphene solution, which is applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of restricting macro-scale preparation applications, low volume density and specific surface area, high resistance and thermal resistance, etc., to achieve Broad application prospects, large specific surface area, and dense pore structure

Active Publication Date: 2016-04-27
FUDAN UNIV
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  • Abstract
  • Description
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Problems solved by technology

However, the size of the graphene foam pore structure obtained by the CVD method is hundreds of microns, and the bulk density and specific surface are very low, which limits its macro preparation and application in some fields.
The aerogel has a denser pore structure with a size of submicron level, but its sheets are in contact with each other through physical interaction, so they have higher electrical resistance and thermal resistance.

Method used

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  • Preparation method of three-dimensional graphene

Examples

Experimental program
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Embodiment 1

[0026] First, the modified Hummers method was used to prepare graphene oxide, and a 5 mg / mL graphene oxide aqueous solution was prepared by mechanical stirring and ultrasound, and poured into an autoclave. The cleaned nickel foam was immersed in the graphene oxide solution. The reactor containing the nickel foam and the graphene oxide solution was left to react at 180° C. for 12 hours to obtain the nickel foam loaded with graphene hydrogel in the pores. The nickel foam loaded with graphene hydrogel was freeze-dried for 3 days to obtain the nickel foam loaded with graphene aerogel ( figure 2 , image 3 ). Take this as a template, put it into a quartz tube, and evacuate it to 5×10 -3 Torr, backfilled with 200 sccm hydrogen and 500 sccm argon to atmospheric pressure. Heat the tube furnace to 1000°C, and anneal at 1000°C for 30 minutes. 10 sccm of methane gas was introduced to grow for 20 minutes. After the growth was over, the samples were taken out after the furnace was c...

Embodiment 2

[0028] First, graphene oxide was prepared by the modified Hummers method, and a 10 mg / mL graphene oxide aqueous solution was prepared by mechanical stirring and ultrasound. According to graphene oxide: ascorbic acid mass ratio is 1:3, adds ascorbic acid to graphene oxide aqueous solution. The cleaned nickel foam was immersed in the graphene oxide / ascorbic acid solution. The graphene oxide / ascorbic acid solution impregnated with nickel foam was left to react at 90° C. for 3 hours to obtain the nickel foam loaded with graphene hydrogel in the pores. The nickel foam loaded with graphene hydrogel was freeze-dried for 3 days to obtain the nickel foam loaded with graphene aerogel. Take this as a template, put it into a quartz tube, and evacuate it to 5×10 -3 Torr, backfilled with 200 sccm hydrogen and 500 sccm argon to atmospheric pressure. Heat the tube furnace to 1000°C, and anneal at 1000°C for 30 minutes. 10 sccm of methane gas was introduced to grow for 20 minutes. After t...

Embodiment 3

[0030] First, graphene oxide was prepared by the modified Hummers method, and a 10 mg / mL graphene oxide aqueous solution was prepared by mechanical stirring and ultrasound. The cleaned nickel foam was immersed in graphene oxide solution, and the graphene oxide solution impregnated with nickel foam was directly freeze-dried for 3 days to obtain nickel foam loaded with graphene airgel. Take this as a template, put it into a quartz tube, and evacuate it to 5×10 -3 Torr, backfilled with 200 sccm hydrogen and 500 sccm argon to atmospheric pressure. The tube furnace was heated to 1000°C at a rate of 2°C / min, and annealed at 1000°C for 30 minutes. Bubble 50 sccm hydrogen / 100 sccm argon into ethanol, use the introduced ethanol vapor as carbon source, and grow for 30 minutes. After the growth was over, the samples were taken out after the furnace was cooled to room temperature. A 4% PMMA anisole solution was added dropwise to the sample surface, followed by curing on a hot stage at ...

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Abstract

The invention belongs to the technical field of preparation of graphene and in particular discloses a preparation method of three-dimensional graphene. The method comprises the following steps: dispersing graphene oxide to obtain a graphene oxide aqueous solution; soaking three-dimensional foams into a graphene oxide solution and obtaining three-dimensional metal foams with graphene aerogels loaded in pores via a physical or chemical method; taking the three-dimensional metal foams with graphene aerogels loaded in pores as templates to obtain substrate-containing three-dimensional graphene via a chemical vapor deposition method; and etching and washing to obtain the three-dimensional graphene. The preparation method of the three-dimensional graphene is simple in process and is capable of preparing high-quality and high-density three-dimensional graphene and laying the foundation of the application of the three-dimensional graphene for the fields of catalysis, energy storage, heat conduction and adsorption.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a preparation method of three-dimensional graphene. Background technique [0002] Graphene is a carbon atom with sp 2 A single-layer honeycomb two-dimensional crystal formed by hybridization. Due to its unique structure and excellent performance, it has become a research hotspot in various disciplines. At present, the methods for preparing graphene are mainly divided into two categories: Top–down and Bottom–up. Top–down methods include: mechanical exfoliation method, redox method, etc. The graphene material obtained by redox method will inevitably introduce structural defects during the preparation process, which will affect its own performance. In contrast, graphene prepared by the Bottom–up method such as chemical vapor deposition has a perfect structure and high quality. However, the yield of these methods for preparing 2D graphene is low, and it is difficult ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/20C01B2204/22C01B2204/32C01P2004/03
Inventor 魏大程亓国强杨伟夏冬云李科李孟林刘冬华曹敏彭兰
Owner FUDAN UNIV
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