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Nitrogen-doped graphene oxide material and preparation method thereof

A nitrogen doping, graphene technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve problems such as unknown impact, achieve the effect of expanding application fields and avoiding irreversible stacking

Active Publication Date: 2014-05-21
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are no international reports on nitrogen-doped graphene oxide, and the effect of nitrogen doping on graphene oxide and corresponding graphene is still unknown.

Method used

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  • Nitrogen-doped graphene oxide material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Take 0.6 g of expanded graphite powder in a crucible, move it to a muffle furnace, and keep it at 400° C. for 0.5 h in an air atmosphere to obtain pre-expanded graphite powder. The obtained graphite powder was dispersed in isopropanol solution, ultrasonicated for 1 h, then 208 μL of pyrrole (Py) was added, stirred vigorously for 0.5 h, 1.3692 g of ammonium persulfate was added for in-situ polymerization for 4 h, and the product was filtered and washed with ethanol and deionized water in sequence After that, it was dried in a vacuum oven at 60°C for 24 hours. The obtained dried samples were calcined at 500° C. for 2 h in an argon (Ar) atmosphere to obtain nitrogen-doped graphite powder. Gained nitrogen-doped graphite powder was added to 80°C containing 30mL of concentrated sulfuric acid, 0.3g potassium persulfate (K 2 S 2 o 8 ) and 0.3g phosphorus pentoxide (P 2 o 5 ) in a round-bottomed flask for 6 h, then cooled to room temperature, the resulting blue solid was wa...

Embodiment 2

[0026]Take 0.6 g of expanded graphite powder in a crucible, move it to a muffle furnace, and keep it at 300° C. for 2 hours in an air atmosphere to obtain pre-expanded graphite powder. The obtained graphite powder was further placed in an argon-ammonia gas mixture with a concentration of 1% and calcined at 700° C. for 48 hours to obtain nitrogen-doped graphite powder. Gained nitrogen-doped graphite powder was added to a condensing reflux device containing 50mL concentrated nitric acid and 32g potassium chlorate (KClO 3 ) solution in a round bottom flask, the temperature was raised to 60° C. for 12 h, and then the product was washed with deionized water. The resulting product was finally dialyzed with a dialysis bag with a molecular weight cut-off of 3500 for 7 days to remove residual ions, and the resulting solution was ultrasonically dispersed to obtain nitrogen-doped graphene oxide.

Embodiment 3

[0028] Take 0.6 g of expanded graphite powder in a crucible, move it to a muffle furnace, and keep it at 500° C. for 3 hours in an air atmosphere to obtain pre-expanded graphite powder. The obtained graphite powder was further placed in 30% helium-ammonia mixed gas and calcined at 1200° C. for 24 hours to obtain nitrogen-doped graphite powder. Gained nitrogen-doped graphite powder was added to 80°C containing 30 mL of concentrated sulfuric acid, 0.3 g of potassium persulfate (K 2 S 2 o 8 ) and 0.3g phosphorus pentoxide (P 2 o 5 ) in a round-bottomed flask for 6 h, then cooled to room temperature, the resulting blue solid was washed and filtered with ultrapure water until the pH was 7, and then dried in a vacuum oven at 50°C, and then the resulting dry solid was slowly added to the In the 50mL concentrated sulfuric acid solution in the water bath, slowly add 4.2g potassium permanganate (KMnO 4 ) and stir until the temperature no longer rises, then keep the reaction tempera...

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Abstract

The invention relates to a nitrogen-doped graphene oxide material and a preparation method thereof. By adopting the material, a part of carbon atoms in graphene oxide are replaced by nitrogen atoms. The preparation method comprises the following steps: firstly, pre-expanding graphite powder, and then obtaining nitrogen-doped graphite powder by doping a nitrogen element into the obtained pre-expanded graphite powder; obtaining nitrogen-doped graphene oxide by using an oxidation-stripping method, and then obtaining the nitrogen-doped graphene oxide material by ultrasonic dispersion. Compared with the prior art, the nitrogen-doped graphene oxide disclosed by the invention not only can be rapidly and cheaply prepared into high-quality graphene by a reduction process under a mild condition, but also can display new characteristics, so as to expand the application field.

Description

technical field [0001] The invention relates to nitrogen-doped graphene oxide, in particular to a nitrogen-doped graphene oxide material and a preparation method thereof. Background technique [0002] Graphene is a new type of carbon allotrope, which consists of carbon atoms arranged in a hexagonal grid to form a two-dimensional structure. It has attracted great attention since it was discovered by K.S. Novoselov and A.K. Geim in 2004 (Science, 306 (2004) 666-669). Graphene has excellent mechanical, electrical, optical and chemical properties, and can be widely used in the fields of nanoelectronic devices, photoelectric conversion and energy storage (Chemical Reviews, 110(2010) 132-145). Usually, graphene is prepared by reducing graphene oxide (Graphene Oxide). For this reason, the application of graphene oxide has been limited to the preparation of graphene. In recent years, graphene oxide has exhibited new properties such as dispersibility, hydrophilicity, and compatibi...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/198
Inventor 马忠原鲜霞李琳马紫峰
Owner SHANGHAI JIAO TONG UNIV
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