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Nitrogen doped graphene material and preparation method thereof

A nitrogen-doped graphene and graphene technology, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve the problems of limited commercial application, high cost, insufficient purity, etc., and achieve easy mass production and increase voltage Value, the effect of high product purity

Active Publication Date: 2012-10-31
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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AI Technical Summary

Problems solved by technology

So far, there are many ways to prepare graphene known, such as: (1) micromechanical exfoliation method; this method can only produce a very limited number of graphene sheets, which can be used as basic research; (2) ultra-high vacuum Graphene epitaxial growth method; the high cost of this method and the structure of small wafers limit its application; (3) chemical vapor deposition (CVD); this method can meet the requirements of large-scale preparation of high-quality graphene, but the cost high, complicated
(4) solvent stripping method; the disadvantage of this method is that the yield is very low, which limits its commercial application; (5) oxidation-reduction method; this method is the simplest and a common method for obtaining graphene in large quantities, and the whole process involves Graphite is oxidized into graphite oxide, and the graphene oxide produced by the exfoliation of graphite oxide is then reduced to graphene by chemical reagents or heat; the final oxygen content of graphene synthesized by this method is high, and the purity is not enough; the existence of oxygen atoms is very important for graphene. The voltage used as the electrode material has a certain influence

Method used

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  • Nitrogen doped graphene material and preparation method thereof
  • Nitrogen doped graphene material and preparation method thereof

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preparation example Construction

[0016] A preparation method of nitrogen-doped graphene material, such as figure 1 shown, including the following steps:

[0017] S1, prepare graphite oxide according to the Hummers method (Hummers WS, Offeman R E.[J].J Am Chem Soc, 1958,80:133921339): 20g of 50 mesh graphite powder with a purity of 99.5%, 10g of potassium persulfate and 10g of five Add phosphorus oxide into concentrated sulfuric acid at 80°C, stir evenly, cool for more than 6 hours, wash until neutral, and dry; add the dried sample to 230mL concentrated sulfuric acid at 0°C, and then add 60g of potassium permanganate, the mixture Keep the temperature below 20°C, then keep it in an oil bath at 35°C for 2 hours, then slowly add 920mL of deionized water; after 15min, add 2.8L of deionized water, then add 50mL of 30wt% hydrogen peroxide solution, and then the mixture The color becomes bright yellow, and it is suction-filtered while it is hot, then washed with 5L of 10% hydrochloric acid, suction-filtered, and vac...

Embodiment 1

[0026] (1) Graphite oxide: Add 20g of 50 mesh graphite powder with a purity of 99.5%, 10g of potassium persulfate and 10g of phosphorus pentoxide into concentrated sulfuric acid at 80°C, stir evenly, cool for more than 6h, wash until neutral, and dry; Add the dried sample to 0°C, 230mL of concentrated sulfuric acid, then add 60g of potassium permanganate, keep the temperature of the mixture below 20°C, then keep it in an oil bath at 35°C for 2h, then slowly add 920mL of deionized water; After 15 minutes, add 2.8L of deionized water, then add 50mL of 30wt% hydrogen peroxide solution, wait until the color of the mixture turns bright yellow, filter while hot, then wash with 5L of 10% hydrochloric acid, filter with suction, Graphite oxide was obtained by vacuum drying at 60°C for 48 hours;

[0027] (2) adding the graphite oxide prepared in (1) into water for ultrasonic dispersion for 0.5h to form a graphene oxide solution uniformly dispersed in a monolithic layer, so that the conc...

Embodiment 2

[0032] (1) the preparation of graphite oxide is the same as in Example 1;

[0033] (2) adding the graphite oxide prepared in (1) into water for ultrasonic dispersion for 1 h to form a graphene oxide solution uniformly dispersed in a monolithic layer, so that the concentration of graphene oxide is 0.1 mg / ml;

[0034] (3) adding mass concentration to the graphene oxide solution in (2) is 10% ammonium bicarbonate solution, stirs 10min, makes both mix uniformly, obtains graphene oxide and ammonium carbonate mixed solution;

[0035] (4) evaporating the solvent from the mixed solution obtained in (3) to obtain a solid mixture;

[0036](5) First raise the temperature of the muffle furnace to 550° C., then put the mixture obtained in (4) into the muffle furnace, keep it for calcination under the protection of a nitrogen atmosphere for 1 h, and cool to obtain a nitrogen-doped graphene material.

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Abstract

The invention belongs to the field of electrochemical materials and discloses a nitrogen doped graphene material and a preparation method thereof. The preparation method of the nitrogen doped graphene material comprises the following steps of: preparing graphite oxidize; preparing graphene oxide solution; preparing mixed solution of graphene oxide and ammonium carbonate; removing solvent in the mixed solution of the graphene oxide and ammonium carbonate; and calcining mixture of graphite oxide and ammonium carbonate, thus obtaining the nitrogen doped graphene oxide material. The nitrogen doped graphene material and preparation method thereof which are disclosed by the invention have the advantages that preparation cost is lower, mass production is easy to realize, product purity is high, ammonium carbonate is completely decomposed into gas at high temperature and no pollution is produced to a product.

Description

technical field [0001] The invention relates to the field of graphene materials, in particular to a nitrogen-doped graphene material. The invention also relates to a preparation method of the nitrogen-doped graphene material. Background technique [0002] Andre K. Geim (Andre K.Geim) of the University of Manchester in the United Kingdom prepared graphene materials in 2004, and it has received widespread attention due to its unique structure and photoelectric properties. Single-layer graphite is considered an ideal material due to its large specific surface area, excellent electrical and thermal conductivity, and low thermal expansion coefficient. Such as: 1, high strength, Young's molar weight, (1,100GPa), breaking strength: (125GPa); 2, high thermal conductivity, (5,000W / mK); 3, high electrical conductivity, carrier transport rate, ( 200,000cm 2 / V*s); 4, high specific surface area, (theoretical calculation value: 2,630m 2 / g). In particular, its high conductivity, lar...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B31/04C01B32/184C01B32/194
Inventor 周明杰钟玲珑王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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