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Preparation method of graphite

A technology of graphene and graphite, which is applied in the field of graphene preparation, can solve the problems of small specific surface area, complex process and high cost of graphene, and achieve the effects of short reaction time, simple process and avoiding agglomeration

Inactive Publication Date: 2013-11-13
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] So far, there are many ways to prepare graphene known, such as: (1) micromechanical exfoliation method, which 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 Higher and complicated process; (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 common method for obtaining graphene in large quantities method, the more commonly used reduction methods are chemical reduction (hydrazine hydrate, ethylenediamine, sodium borohydride, etc. as reducing agents) and rapid thermal reduction, but after various methods of reduction, graphene will have a reunion process, resulting in graphene The specific surface area is small, generally less than 700m 2 / g

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  • Preparation method of graphite

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Embodiment 1

[0030] A method for preparing graphene, comprising the steps of:

[0031] (1) Preparation of graphite oxide:

[0032] Get the graphite that purity is 99.5% and prepare graphite oxide, its concrete steps are:

[0033] Add 20g of 50-mesh graphite, 10g of potassium persulfate and 10g of phosphorus pentoxide into concentrated sulfuric acid at 80°C, stir evenly, cool for 6h, wash until neutral, and dry; add the dried sample to 230mL of concentrated sulfuric acid at 0°C Add 60g of potassium permanganate, keep the temperature of the mixture at 20°C, then keep it in an oil bath at 35°C for 2h, then slowly add 920mL of deionized water; after 15min, add 2.8L of deionized water (which contains 50mL of 30% hydrogen peroxide), after which the color of the mixture turned bright yellow, suction filtered while hot, then washed with 5L of 10% hydrochloric acid, suction filtered, and vacuum dried at 60°C for 48 hours to obtain graphite oxide.

[0034] (2) Drying: the obtained graphite oxide w...

Embodiment 2

[0039] A method for preparing graphene, comprising the steps of:

[0040] (1) Preparation of graphite oxide:

[0041] Get the graphite that purity is 99.5% and prepare graphite oxide, its concrete steps are:

[0042] Add 20g of 50-mesh graphite, 10g of potassium persulfate and 10g of phosphorus pentoxide into concentrated sulfuric acid at 80°C, stir evenly, cool for 7 hours, wash until neutral, and dry; add the dried sample to 230mL of concentrated sulfuric acid at 0°C Add 60g of potassium permanganate, keep the temperature of the mixture at 18°C, then keep it in an oil bath at 35°C for 2h, then slowly add 920mL of deionized water; after 15min, add 2.8L of deionized water (which contains 50mL of 30% hydrogen peroxide), after which the color of the mixture turned bright yellow, suction filtered while hot, then washed with 5L of 10% hydrochloric acid, suction filtered, and vacuum dried at 60°C for 48 hours to obtain graphite oxide.

[0043] (2) Drying: the obtained graphite ox...

Embodiment 3

[0047] A method for preparing graphene, comprising the steps of:

[0048] (1) Preparation of graphite oxide:

[0049] Get the graphite that purity is 99% and prepare graphite oxide, its specific steps are:

[0050] Add 20g of 50-mesh graphite, 10g of potassium persulfate and 10g of phosphorus pentoxide into concentrated sulfuric acid at 80°C, stir evenly, cool for 8 hours, wash until neutral, and dry; add the dried sample to 230mL of concentrated sulfuric acid at 0°C Add 60g of potassium permanganate, keep the temperature of the mixture at 16°C, then keep it in an oil bath at 35°C for 2h, then slowly add 920mL of deionized water; after 15min, add 2.8L of deionized water (which contains 50mL of 30% hydrogen peroxide), after which the color of the mixture turned bright yellow, suction filtered while hot, then washed with 5L of 10% hydrochloric acid, suction filtered, and vacuum dried at 60°C for 48 hours to obtain graphite oxide.

[0051] (2) Drying: The obtained graphite oxid...

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Abstract

The invention provides a preparation method of graphite. The method comprises the following steps: carrying out high temperature reduction on graphite oxide under protection of inert gas at 800-1200 DEG C for 10-60 s; transferring the high temperature reduction products to liquid nitrogen, and cooling for 3-30 s; and after cooling, collecting a black powder namely the prepared graphite. In the method, huge temperature difference between high temperature reduction and liquid nitrogen refrigeration makes the graphite wrinkle more easily, thereby effectively avoiding agglomeration among sheet layers of the graphite. The graphite prepared by the method provided by the invention has a high specific surface area reaching 700-1500 m<2> / g. In addition, the method has simple process and short reaction time.

Description

technical field [0001] The invention relates to the field of material synthesis, in particular to a method for preparing graphene. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004. It is a single-layer or multi-layer extremely thin carbon material. Single-layer graphene 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), fracture 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). Among them, graphene's high conductivity, large specific surface properties and its two-dimensional nanoscale structural properties of monomolecular layers enable graphene...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184C01B32/186
Inventor 周明杰钟玲珑王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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