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Surface porous graphene material and preparation method thereof

A surface porous and graphene technology, applied in the field of nanomaterials, can solve the problem of low controllability of nanopore size and surface distribution density, low controllability of ablated pore size and density, and nanoparticle size and density. Uncontrollable load efficiency and other problems, to achieve the effect of uniform surface loaded oxide, short preparation time and low equipment requirements

Inactive Publication Date: 2016-07-20
TAISHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are three main preparation methods for corroding holes on the surface of graphene: the first method is concentrated nitric acid and potassium permanganate and other oxidant oxidation methods. The disadvantages of this type of method are the use of concentrated acid, washing with a large amount of water or Dialysis, the size and distribution density of surface pores are not controllable; the second method is the oxide surface ablation method, which requires the deposition of oxide nanoparticles on the surface of graphene
The technique of ex-situ deposition of nanoparticles makes the size and loading efficiency of nanoparticles uncontrollable, thus leading to a low degree of controllability of the size and density of the ablated pores
In addition, the in-situ deposition of oxide nanoparticles technology is also carried out in aqueous solution, which inevitably leads to irregular growth of nanoparticles. Therefore, the controllability of the size of nanopores and surface distribution density is not high.
In addition, a precipitating agent is required in the precipitation reaction, thus, cumbersome washing steps are required in the subsequent processing
The third approach is a bottom-up chemical and high-energy technological approach through aryl-aryl coupling reactions, which are generally prepared on substrates with low yields
For example, the porous graphene in patent application CN104959134A and CN104934574A is ultrasonically obtained in concentrated nitric acid solution, and a large amount of concentrated acid is used in the preparation process, so cumbersome centrifugation and washing steps are required
In the preparation method of a porous graphene material described in the patent CN102107868A, non-situ technology is used to deposit nanoparticles on the surface of graphene. Since the size and loading efficiency of nanoparticles are uncontrollable, the size of the ablated pores and Density controllability is not high

Method used

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  • Surface porous graphene material and preparation method thereof

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Effect test

Embodiment 1

[0031] Disperse 2 mg of graphene oxide in 10 ml of ethanol, sonicate until the solution is evenly dispersed and translucent light brown, add 8 mg of nickel nitrate and stir to dissolve it completely. Add 5 grams of solid carbon dioxide (dry ice) to the above solution, place the above mixture in a 100 ml autoclave, heat and react at 200°C for 0.5 hour while stirring; cool, centrifuge, and dry the reacted solution in an inert Calcining at 800° C. for 1 hour in an atmosphere (nitrogen) to obtain graphene with nanopores on the surface. Such as figure 1 As shown, the pores on the surface of the porous graphene material are evenly distributed, and the nanopore diameters are concentrated in the range of 80-150nm.

Embodiment 2

[0033] Disperse 30 mg of graphene oxide in 20 ml of methanol, sonicate until the solution is uniformly dispersed and translucent light brown, then add 60 mg of copper nitrate and stir. Add 4 grams of solid carbon dioxide (dry ice) to the above solution, place the above mixture in a 100 ml autoclave, heat and react at 170°C for 0.8 hours while stirring; cool, centrifuge, and dry the reacted solution in an inert Calcining at 600° C. for 1 h in an atmosphere (argon gas) to obtain graphene with nanopores on the surface. The pores on the surface of the porous graphene material are evenly distributed, and the diameters of the nanopores are concentrated in the range of 100-200 nm.

Embodiment 3

[0035] Disperse 200 mg of graphene oxide in 40 ml of acetonitrile, sonicate until the solution is uniformly dispersed and translucent light brown, add 100 mg of ferric nitrate and stir to dissolve it completely. Add 5 grams of solid carbon dioxide (dry ice) to the above solution, place the above mixture in a 200 ml autoclave, heat and react at 180° C. for 1 hour while stirring; cool, centrifuge, and dry the reacted solution in an inert Calcining at 900° C. for 0.5 h in an atmosphere (argon gas) to obtain graphene with nanopores on the surface. The pores on the surface of the porous graphene material are evenly distributed, and the diameters of the nanopores are concentrated in the range of 50-100 nm.

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Abstract

The invention discloses a surface porous graphene material and a preparation method thereof. The preparation method comprises the following steps: (1) dispersing a graphene material in a cosolvent in an ultrasonic dispersion manner till a solution is uniformly dispersed and is semitransparent and bright brown; (2) adding metallic nitrate into the solution obtained in the step (1), and stirring till the metallic nitrate is completely dissolved; (3) adding solid carbon dioxide into the solution obtained in the step (2); (4) enabling the solution obtained in the step (3) to be subjected to heating reaction in a sealed container, cooling the solution obtained after reaction, centrifuging, drying, and collecting a solid product; (5) calcining the solid product obtained in the step (5) in inert atmosphere, so as to obtain the surface porous graphene material. The preparation method disclosed by the invention is simple, easily obtainable in raw material, low in equipment requirement, simple to operate, high in reaction speed, short in preparation time, free of pollution and energy-saving and environment-friendly, and the prepared surface porous graphene material is uniform and controllable in surface pore distribution, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to a surface porous graphene material and a preparation method thereof. Background technique [0002] In 2004, the research team of Professor Andre Geim of the University of Manchester used a mechanical exfoliation method to obtain graphene with a single atomic layer thickness, and measured their physical properties - the Hall effect. As a result, they were awarded the 2010 Nobel Prize in Physics. The good properties and application prospects of graphene have attracted great attention in the fields of scientific research and application. Graphene-loaded composite oxides are one of the many research fields in graphene composites. Among the above composites, graphene has high electrical conductivity, specific surface area, good chemical stability and mechanical properties, making the obtained composites The overall electrical conductivity and machining performance of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2004/03C01P2006/17
Inventor 禚林海张金军
Owner TAISHAN UNIV
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