Preparing method for three-dimensional nanometer porous graphene

A porous graphene, nanoporous technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the rare research results of three-dimensional graphene with nanoscale pore structure and controllable pore structure problems such as poor reproducibility and repeatability, performance discount of 3D graphene, etc., to achieve the effect of low cost, cost saving and simplified process flow

Inactive Publication Date: 2016-01-06
TIANJIN UNIV
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Problems solved by technology

[0004] (1) The above methods all rely on reduced graphene oxide (rGO) as a raw material, and there is a large gap between the conductivity of rGO and the ideal two-dimensional graphene. Therefore, the properties of three-dimensional graphene obtained by the above methods will be Big discount
[0005] (2) rGO nanosheets are very easy to re-accumulate and agglomerate in the process of forming a three-dimensional graphene structure. How to maintain the sheet properties of rGO intact is still a difficult point;
[0006] (3) The microscopic pore structure of the three-dimensional graphene material assembled by rGO nanosheets mostly appears randomly during the integration process of 2D graphene, and the controllability and repeatability of the pore structure are poor;
[0007] (4) The pore size of the three-dimensional graphene obtained by the above methods has exceeded the nanometer level, which is not a true three-dimensional nanoporous graphene
[0008] Chemical vapor deposition (CVD) is currently the most effective method for preparing high-quality graphene, so it is also the most effective method for preparing three-dimensional nanoporous graphene. However, the pore size of three-dimensional graphene materials prepared by CVD is usually in the range of several Between hundreds of nanometers and tens of microns, but there are still few research results on three-dimensional graphene with nanoscale pore structure

Method used

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  • Preparing method for three-dimensional nanometer porous graphene
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  • Preparing method for three-dimensional nanometer porous graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Choose Cu with a thickness of 50um 30 mn 70 Alloy foil and cut it into 1*1cm 2 size. Then configure a hydrochloric acid solution with a concentration of 0.05M, immerse the alloy foil in the hydrochloric acid solution, and carry out dealloying at room temperature. The dealloying time is 120 minutes. After dealloying, the foil is passed through deionized water-alcohol After cleaning, put it into a vacuum drying oven after cleaning, and vacuum dry at room temperature for 12 hours to obtain nanoporous copper. Put the completely dry nanoporous copper into the quartz ark, and place the ark in the outer area of ​​the reaction tube furnace, and feed acetylene, argon and hydrogen, and the ratio of the three gases is C 2 h 2 :Ar:H 2 =5:500:200 sccm. At the same time, the temperature of the tube furnace was raised to 800°C. When the furnace temperature reached 800°C, the quartz ark was quickly moved from the outside of the furnace to the constant temperature zone in the midd...

Embodiment 2

[0032] Choose Cu with a thickness of 150um 30 mn 70 Alloy foil and cut it into 1*2cm 2size. Then an ammonium sulfate solution with a concentration of 1M was prepared, and the alloy was dealloyed by a constant potential method at room temperature with a corrosion potential of -0.4V and a corrosion time of 150 minutes. After dealloying, the foils were cleaned by deionized water-alcohol in sequence, put into a vacuum drying oven after cleaning, and vacuum-dried at room temperature for 12 hours to obtain nanoporous copper. Put the completely dried nanoporous copper into the quartz ark, place the ark in the outer area of ​​the reaction tube furnace, and feed methane, argon and hydrogen, and the ratio of the three gases is C 2 h 2 :Ar:H 2 =20:500:200 sccm. At the same time, raise the temperature of the tube furnace to 900°C. When the furnace temperature reaches 900°C, quickly move the quartz ark from the outside of the furnace to the constant temperature zone in the middle of ...

Embodiment 3

[0034] Choose Ni with a thickness of 100um 15 Cu 15 mn 70 Alloy foil, and cut it into 2*1cm 2 size. Then an ammonium sulfate solution with a concentration of 1M was prepared, and the alloy was dealloyed by a constant potential method at room temperature, with a corrosion potential of -0.5V and a corrosion time of 240 minutes. After de-alloying, the foils are cleaned by deionized water-alcohol in sequence, put into a vacuum drying oven after cleaning, and vacuum-dried at room temperature for 12 hours to obtain nanoporous nickel-copper. Put the completely dried nano-porous nickel-copper into the quartz ark, and place the ark in the outer area of ​​the reaction tube furnace, and feed ethylene, argon and hydrogen, and the ratio of the three gases is C 2 h 4 :Ar:H 2 = 1:200:50 sccm. At the same time, raise the temperature of the tube furnace to 1000°C. When the furnace temperature reaches 1000°C, quickly move the quartz ark from the outside of the furnace to the constant tem...

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Abstract

The invention provides a preparing method for three-dimensional nanometer porous graphene. The preparing method includes the following steps that Cu-Mn alloy foil is prepared; dealloying treatment is carried out, and nanometer porous copper foil is obtained; the three-dimensional nanometer porous graphene is prepared, wherein the temperature rises to 200 DEG C to 400 DEG C in argon and hydrogen atmosphere, acetylene is introduced to grow hydrogenated graphite, the furnace temperature rises to 500 DEG C to 1,100 DEG C in hydrogen atmosphere, a quartz boat is rapidly moved to a temperature constant region in the middle of a reaction pipe to be roasted after the furnace temperature rises to the assigned temperature, the sample is cooled to the indoor temperature in hydrogen atmosphere after roasting is completed, the sample is immersed into corrosive fluid to remove nanometer porous copper, and a self-supporting three-dimensional nanometer porous graphene film is obtained after washing. According to the preparing method, the technological process is simple, cost is low, the pore sizes of the obtained three-dimensional nanometer porous graphene are even in distribution and are all in the nanometer level, and the obtained three-dimensional nanometer porous graphene is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanomaterials, and in particular relates to a preparation method of three-dimensional nanoporous graphene. Background technique [0002] Graphene is a single-layer two-dimensional carbonaceous material formed by densely packed carbon atoms, and its theoretical specific surface area reaches 2620m 2 / g, and has excellent electrical, optical, mechanical and other properties, so it has a very wide application prospect. At present, graphene and its functionalized derivatives can be prepared by mechanical exfoliation, epitaxial growth, chemical vapor deposition, and chemical reduction. Integrating two-dimensional graphene to construct graphene with a specific three-dimensional structure, and then preparing functional devices with excellent performance are of great significance for expanding the macroscopic application of graphene. The three-dimensional structure can endow graphene with unique p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y30/00
Inventor 李家俊秦凯强康建立赵乃勤何春年刘恩佐师春生
Owner TIANJIN UNIV
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