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Preparation method of graphene

A technology of graphene and graphene suspension, applied in the direction of graphene, nano-carbon, etc., can solve the problem of high oxygen content in graphene

Active Publication Date: 2014-01-15
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the theoretical specific surface area of ​​graphene is as high as 2600m 2 / g, but the specific surface area of ​​graphene prepared by the general method is generally 600m 2 / g, which is much lower than its theoretical specific surface area, and the prepared graphene has a higher oxygen content

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preparation example Construction

[0026] see figure 1 , the preparation method of the graphene of one embodiment, comprises the steps:

[0027] Step S110, preparing graphite oxide.

[0028] Preparation of graphite oxide comprises the following steps:

[0029] Step 1. Add graphite to the mixed acid solution composed of concentrated sulfuric acid and concentrated nitric acid to form a mixed solution, keep the temperature of the mixed solution at -2°C~2°C and stir for 10min~30min.

[0030] Preferably, the purity of graphite is 99.5%. Graphite is a powder with a particle size in the order of microns.

[0031] Preferably, the solid-to-liquid ratio of graphite to concentrated sulfuric acid and concentrated nitric acid is 1g:(80ml~110ml):(15ml~35ml).

[0032] Preferably, the mixed solution is placed in an ice-water bath and stirred for 20 minutes.

[0033] Preferably, the mass concentration of concentrated nitric acid is 98%, and the mass concentration of concentrated nitric acid is 65%.

[0034] Step 2: Add po...

Embodiment 1

[0063] Present embodiment is by graphite oxide, and the process flow diagram of preparing graphene through exfoliation and electrochemical and chemical co-reduction is as follows:

[0064] Graphite → graphite oxide → graphene oxide → graphene

[0065] (1) Graphite: 99.5% purity;

[0066](2) Graphite oxide: Weigh 1g of graphite with a purity of 99.5% in (1) and add it to a mixed solution consisting of 90ml of concentrated sulfuric acid (98% by mass fraction) and 25ml of concentrated nitric acid (65% by mass fraction). Place in an ice-water mixed bath environment and stir for 20 minutes, then slowly add 6g of potassium permanganate to the mixture, stir for 1 hour, then heat the mixture to 85°C and keep it for 30 minutes, then add 92ml of deionized water Continue to keep at 85°C for 30 minutes, finally add 10ml of hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, and then use 100ml of dilute hydrochloric acid and 150ml of deion...

Embodiment 2

[0074] Present embodiment is by graphite oxide, and the process flow diagram of preparing graphene through exfoliation and electrochemical and chemical co-reduction is as follows:

[0075] Graphite → graphite oxide → graphene oxide → graphene

[0076] (1) Graphite: 99.5% purity;

[0077] (2) Graphite oxide: Weigh 5g of graphite with a purity of 99.5% in (1) and add it to a mixed solution consisting of 475ml of concentrated sulfuric acid (98% by mass fraction) and 120ml of concentrated nitric acid (65% by mass fraction). Place in an ice-water mixed bath environment and stir for 20 minutes, then slowly add 20g of potassium permanganate to the mixture, stir for 1 hour, then heat the mixture to 85°C and keep it for 30 minutes, then add 92ml of deionized water Continue to keep at 85°C for 30 minutes, finally add 30ml of hydrogen peroxide solution (mass fraction 30%), stir for 10 minutes, filter the mixture with suction, and then use 300ml of dilute hydrochloric acid and 450ml of d...

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Abstract

A preparation method of graphene comprises the following steps: adding graphite oxide into water for ultrasonic dispersion to form a graphene oxide suspension, and filtering to obtain graphene oxide; dispersing the graphene oxide and a reducing agent in a solution containing an electrolyte to form an electrolytic solution, wherein the reducing agent being at least one selected from sodium borohydride and hydrazine hydrate, and the electrolyte being at least one selected from the group consisting of sodium chloride, sodium nitrate and potassium chloride; using a copper plate as a cathode and a platinum rod as an anode, regulating the electrolytic solution temperature to 70DEG C-90 DEG C, under the conditions of the voltage of 0.8V-1.5V, electrolyzing the electrolytic solution for 0.5 hour to 2 hours to obtain the graphene on the surface of the cathode. The graphene prepared by the preparation method is large in specific surface area and low in oxygen content.

Description

technical field [0001] The invention relates to a preparation method of graphene. Background technique [0002] Graphene is a two-dimensional monolayer material with excellent physical properties, such as high theoretical specific surface area, excellent mechanical strength, good flexibility and high electrical conductivity, etc., and has attracted extensive attention from researchers. Although the theoretical specific surface area of ​​graphene is as high as 2600m 2 / g, but the specific surface area of ​​graphene prepared by the general method is generally 600m 2 / g, which is far below its theoretical specific surface area, and the prepared graphene has a relatively high oxygen content. Contents of the invention [0003] Based on this, it is necessary to provide a preparation method of graphene with larger specific surface area and lower oxygen content. [0004] A kind of preparation method of graphene, comprises the steps: [0005] adding graphite oxide into water to...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/19
Inventor 周明杰钟辉王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD