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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  • Abstract
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  • Application Information

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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

Method used

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Example Embodiment

[0016] A method for preparing nitrogen-doped graphene materials, such as figure 1 As shown, including the following steps:

[0017] S1. According to the Hummers method (Hummers WS, Offeman R E. [J]. J Am Chem Soc, 1958, 80: 133921339) to prepare graphite oxide: 20g of 50 mesh graphite powder with a purity of 99.5%, 10g of potassium persulfate and 10g of five Phosphorus oxide was added to concentrated sulfuric acid at 80°C, stirred uniformly, cooled for more than 6 hours, washed to neutrality, and dried; the dried sample was added to 230mL concentrated sulfuric acid at 0°C, and then 60g potassium permanganate was added. Keep the temperature below 20℃, then keep it in the oil bath at 35℃ for 2h, slowly add 920mL deionized water; 15min later, add 2.8L deionized water, and then add 50mL 30wt% hydrogen peroxide solution, then the mixture The color becomes bright yellow, and it is filtered while it is hot, and then washed with 5L of 10% hydrochloric acid, filtered by suction, and dried...

Example Embodiment

[0025] Example 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 6 hours, wash to neutrality, and dry; The dried sample was added to 0℃, 230mL concentrated sulfuric acid, and then 60g potassium permanganate was added. The temperature of the mixture was kept below 20℃, and then kept in an oil bath at 35℃ for 2h, then 920mL deionized water was slowly added; After 15 minutes, add 2.8L of deionized water, and then add 50mL of 30wt% hydrogen peroxide solution. When the color of the mixture turns to bright yellow, it is filtered while hot, and then washed with 5L of 10% hydrochloric acid. Vacuum drying at 60°C for 48 hours to obtain graphite oxide;

[0027] (2) Add the graphite oxide prepared in (1) to water and ultrasonically disperse for 0.5h to form a graphene oxide solution uniformly dispersed in a single layer, ...

Example Embodiment

[0031] Example 2

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

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

[0034] (3) Add ammonium bicarbonate solution with a mass concentration of 10% to the graphene oxide solution in (2), stir for 10 minutes to mix the two uniformly, and obtain a graphene oxide and ammonium carbonate mixed solution;

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

[0036] (5) First heat the muffle furnace to 550° C., and then put the mixture obtained in (4) into the muffle furnace, heat and calcinate for 1 h under the protection of a nitrogen atmosphere, 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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