Method for efficiently preparing pore size controllable three-dimensional graphene

A graphene and graphene dispersion technology, which is applied in the field of graphene oxide and three-dimensional graphene preparation and its pore structure control, can solve the problems of high energy consumption, high cost, and high quality of three-dimensional graphene, and achieve high efficiency, The effect of simple operation and low cost

Active Publication Date: 2014-11-26
SOUTHEAST UNIV
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

The three-dimensional graphene prepared by self-assembly of graphene oxide precursor is often difficult to form a uniform and coordinated three-dimensional network, the macroscopic structure is disordered, and its pore size and shape are difficult to control, which hinders its electrical properties to a certain extent. Improve and optimize the three-dimensional structure; while the CVD method uses carbon-containing gas as the carbon source and metal foam as the substrate to grow graphene at high temperature. The three-dimensional graphene prepared by this method is of high quality, but the energy consumption is large and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0014] A. Preparation of graphene oxide:

[0015] Add graphite powder into a three-neck flask in ice bath, add 80-120ml of 98%wt concentrated sulfuric acid, stir for 5-15 minutes, then add 0.2-1g of sodium nitrate. After 10-30 minutes of reaction, potassium permanganate was added and stirred for 30-70 minutes. Then raise the temperature to about 40-60°C and react for 4-8 hours, then add 40-100ml deionized water. After the solution is cooled, the product is centrifugally cleaned to obtain graphite oxide. The obtained graphite oxide sol is ultrasonically peeled for 0.5-2 hours to obtain a light brown graphene oxide dispersion, and the required concentration is prepared.

[0016] B. Preparation of three-dimensional graphene oxide:

[0017] Cut the foam metal copper with the required pore size into a circular template matching the diameter of the Buchner funnel of the suction filtration device, soak it in 30-50%wt dilute hydrochloric acid (HCl) for 20-50s to remove the surface ...

Embodiment 1

[0024] (1). Add 0.5-2g of graphite powder into a three-neck flask in ice bath, add 80-120ml of 98%wt concentrated sulfuric acid, stir for 5-15 minutes, then add 0.1-1g of sodium nitrate. After reacting for 10-30 minutes, add 2-5 g of potassium permanganate and stir for 30-80 minutes. Then raise the temperature to about 40-60°C and react for 3-8 hours, then add 70-100ml deionized water. After the solution is cooled, the product is centrifugally cleaned to obtain graphite oxide. The obtained graphite oxide sol was exfoliated by ultrasonication for 0.5-1.5 hours to obtain a light brown graphene oxide dispersion liquid, which was prepared into a colloid of 3-10 mg / ml.

[0025] (2). Take foam copper with a pore size of 1200 μm, cut it into a circle (d=5-15cm) with the size of the Buchner funnel in the suction filter device, soak it with 30-50% wt dilute hydrochloric acid (HCl) for 20-60 Seconds later, wash it thoroughly with deionized water, dry it, put it into a funnel covered w...

Embodiment 2

[0031] (1). Same as scheme 1, process (1).

[0032] (2). Take foamed copper with a pore size of 800 μm and cut it into a circle of the size of the Buchner funnel in the suction filtration device.

[0033] (d=5-15cm), with the dilute hydrochloric acid (HCl) of 30-50%wt (HCl) immerse 20-60 second and thoroughly clean with deionized water, put into the funnel that has laid filter paper after airing, pour 50- Suction filtration after 150ml graphene oxide dispersion liquid.

[0034] (3). Immerse the completely drained intermediate product in polymethyl methacrylate (950PMMA) for 0.5-3 minutes, take it out and dry it at 80-150°C.

[0035](4). Put the intermediate product coated with polymethyl methacrylate (950PMMA) into 100ml, 25-40% wt of hydroiodic acid (HI) solution at the backlight, and react for 0.5-1.5 hours.

[0036] (5). The material in step (4) is taken out, thoroughly cleaned with deionized water and soaked in 100ml, 0.1mol / L ammonium persulfate ((NH4) 2 S 2 o 8 ) so...

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PUM

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Abstract

The invention provides a method for attaching graphene to foamed metal copper framework through vacuum filtration to control the pore size structure of three-dimensional graphene, which mainly comprises the following processing steps: 1, placing foamed metal copper into a Buchner funnel with spread filter paper, pouring graphene oxide dispersion liquid, and performing vacuum filtration; and 2, coating a polymethyl methacrylate (PMMA) layer on the obtained intermediate compound, reducing with hydriodic acid, immersing in a ammonium persulfate solution to remove the foamed copper framework, then placing in a pipe furnace, introducing argon and hydrogen mixed gas to perform further reduction, and removing the polymethyl methacrylate (PMMA). The process flow is simple and easy to operate, stable in process and low in cost, and can control the pore size and morphological structure of the three-dimensional graphene, thus providing a method for efficiently and stably preparing porous three-dimensional graphene and controlling the pore size thereof; the structural three-dimensional network of the product is continuous and uniform; and the product has favorable adsorbability and electrical conductivity, and has wide application prospects in the aspects of water treatment and electrochemistry.

Description

technical field [0001] The invention relates to the preparation of graphene oxide and three-dimensional graphene and a method for controlling the pore structure thereof, belonging to the technical field of material chemical preparation. Background technique [0002] Graphene is a new type of carbon nanomaterial, which has a two-dimensional honeycomb crystal structure formed by densely packed single-layer carbon atoms. The perfect lattice structure makes it have excellent and unique mechanical, electrical, optical and thermal properties. Including high thermal conductivity, ultra-high electron mobility at room temperature, high theoretical specific surface area, etc., so that it has a wide range of application potential in quantum devices such as field effect transistors, integrated circuits, functional composite materials, energy storage materials, catalyst carriers, etc. . Graphene can be regarded as a two-dimensional macromolecule, and there are many dangling bonds on the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 郭新立李琦张灵敏王蔚妮郝威张艳娟
Owner SOUTHEAST UNIV
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