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Preparation method of nitrogen doped graphene/ metal oxide nanometer composite material

A technology of nitrogen-doped graphene and nanocomposite materials, which is applied in the direction of titanium oxide/hydroxide, oxides of ferrous iron, chemical instruments and methods, etc., can solve the problems of complex preparation process, large pollution, high cost, etc. Achieve the effect of simple process, less equipment investment and short cycle

Active Publication Date: 2012-07-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method of synthesizing nitrogen doping is generally arc discharge or chemical vapor deposition. The preparation process of these methods is complicated, high in cost, and polluting, and it is difficult to prepare in large quantities.

Method used

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  • Preparation method of nitrogen doped graphene/ metal oxide nanometer composite material
  • Preparation method of nitrogen doped graphene/ metal oxide nanometer composite material
  • Preparation method of nitrogen doped graphene/ metal oxide nanometer composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 7.7 g of titanium chloride (TiCl 4 ) and 1 g of graphene were poured into a container filled with ethanol and ultrasonically dispersed for 15 h to obtain a mixture. Then this mixed solution is poured in airtight container A, communicates with another airtight container B that ammoniacal liquor is filled, at 130 o C, the volatilized ammonia gas reacted with titanium chloride at the gas-liquid interface for 6 h, cooled, centrifuged, washed, dried, and finally put the dried powder into a tube furnace, and passed ammonia gas for 800 o C, 6 h, lowered to room temperature to obtain nitrogen-doped graphene / TiO 2 The yield of the nanocomposite material was 94.62%, and the percentage of nitrogen-doped graphene in the obtained composite material was 19.49 wt%.

[0030] The X-ray diffraction pattern of gained composite material and transmission electron microscope are respectively as follows figure 2 and image 3 As shown, it can be seen that the resulting composite is ...

Embodiment 2

[0033] Weigh 20 g bismuth nitrate (Bi(NO 3 ) 3 ·5H 2 O) and 1 g of graphene were poured into a container filled with N, N-dimethylformamide, and ultrasonically dispersed for 6 h to obtain a mixed solution. Then pour the mixed solution into the airtight container A and communicate with another airtight container B containing ammonia water. At 150°C, the volatilized ammonia gas reacts with bismuth nitrate at the gas-liquid interface for 3 hours, cools, centrifuges, Wash, dry, and finally put the dried powder into a tube furnace, pass a mixture of ammonia and argon at 800 °C for 2 h, and cool down to room temperature to obtain nitrogen-doped graphene / Bi 2 o 3 Nanocomposite material, the yield rate is 91.69%, and the percentage of nitrogen-doped graphene in the obtained composite material is 4.03 wt%.

[0034] The X-ray diffraction patterns and transmission electron micrographs of the resulting composite material show that the resulting composite material is nitrogen-doped gra...

Embodiment 3

[0037] Weigh 7.7 g tin chloride (SnCl 4 ·5H 2 O) and 1 g of graphene, poured into a container filled with ethylene glycol, and ultrasonically dispersed for 8 h to obtain a mixed solution. Then pour the mixed solution into the airtight container A, and communicate with another airtight container B containing ammonia water. At 200°C, the volatilized ammonia gas reacts with tin chloride at the gas-liquid interface for 9 hours, then cools and centrifuges. , washing, drying, and finally put the dried powder into a tube furnace, pass ammonia gas at 700 °C for 5 h, and cool down to room temperature to obtain nitrogen-doped graphene / SnO 2 The yield of the nanocomposite material was 96.17%, and the percentage of nitrogen-doped graphene in the obtained composite material was 22.76 wt%.

[0038] The X-ray diffraction patterns and transmission electron microscope photos of the obtained composite material show that the obtained composite material is nitrogen-doped graphene / SnO 2nanocomp...

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Abstract

The invention discloses a preparation method of a nitrogen doped graphene / metal oxide nanometer composite material. The preparation method comprises the following steps of: weighing graphene and metal salt the cation of which is trivalent or quadrivalent to be added in a dispersant, and then carrying out ultrasonic dispersion to obtain mixed liquor; (2), reacting the mixed liquor obtained in the step (1) with alkaline air on a gas-liquid interface for 3-12hours at the temperature of 60-200 DEG C, cooling, centrifuging, washing a precipitate and drying to obtain powder; and (3) introducing the alkaline air or a mixed gas of the alkaline air and inert gas, maintaining the powder to be at the constant temperature of 600-900 DEG C for 2-6 hours, and cooling to room temperature to obtain the nitrogen doped graphene / metal oxide nanometer composite material. According to the invention, the conductibility and interface action of the composite material obtained by the method provided by the invention are improved due to the doping of nitrogen; and the method provided by the invention has the advantages of simple process, cheap cost, high productive rate, short cycle and the like, and is environment-friendly, and can be suitable for industrialization large-scale production.

Description

technical field [0001] The invention relates to the field of nanocomposite materials, in particular to a method for preparing a nitrogen-doped graphene / metal oxide nanocomposite material. Background technique [0002] Graphene with a two-dimensional structure has high thermal conductivity, good mechanical properties, excellent electronic conductivity and large specific surface area, and has important application value in lithium-ion batteries, supercapacitors, photocatalysis and other fields. However, graphene is prone to agglomeration when it exists alone. People hope to overcome the agglomeration between graphene interfaces and solve the problems of low conductivity and volume expansion of metal oxides by preparing graphene / metal oxide composites. However, most of the synthesized graphene has unnecessary functional groups, and since graphene is a two-dimensional open system, it is difficult for metal oxides to be tightly fixed on graphene sheets, so that metal particles an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01G23/053C01G29/00C01G19/02C01G49/08C01G30/00C01G51/04B82Y30/00B82Y40/00C01B32/194
Inventor 王海辉蔡丹丹廉培超梁树钊
Owner SOUTH CHINA UNIV OF TECH
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