Method for preparing graphene

A graphene, graphene powder technology, applied in graphene, nanotechnology, nanocarbon and other directions, can solve the problems of violent reaction, affecting the physical and chemical properties of graphene, easy to increase graphene, etc., to achieve mild reaction conditions, reduce Defect generation, effect of improving purity

Inactive Publication Date: 2012-07-04
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prior to the present invention, previous work mainly used hydrazine hydrate and its derivatives as reducing agents to reduce graphene oxide, but hydrazine hydrate and its derivatives are highly toxic and volatile, and cannot be used on a large scale , and the reduced graphene will be doped with many nitrogen atoms, which will affect the physical and chemical properties of graphene
In the last two years, there have also been reports in the literature that the use of sodium borohydride (NaBH 4 ), ascorbic acid (VC), etc. as reducing agents to reduce graphene oxide, but these reactions require heating, the reaction is more violent, and it is easy to increase the defects of graphene

Method used

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  • Method for preparing graphene
  • Method for preparing graphene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Washing and purifying graphene oxide:

[0022] Dissolve 10mg of graphene oxide into 10ml of water, ultrasonically disperse and dissolve, then centrifuge and wash with 3% HCl and deionized water at 20,000 rpm for 3 times, add deionized water to obtain a uniform 1mg / ml Graphene oxide aqueous solution;

[0023] (2) Add CuCl 2 Solution:

[0024] 100ul of 1mM CuCl 2 Add the solution into the graphene oxide aqueous solution, stir and mix evenly.

[0025] (3) Reduced graphene oxide:

[0026] Add 20mgNaBH 4 , stirred and mixed evenly, and reacted for 6 hours.

[0027] (4) washing and purifying graphene:

[0028] At 10,000 rpm, they were washed by centrifugation with 3% HCl and deionized water for 6 times, and vacuum-dried at 60°C to obtain graphene powder.

[0029]

Embodiment 2

[0031] (1) washing and purification:

[0032] Dissolve 10mg of graphene oxide into 10ml of water, ultrasonically disperse and dissolve, then centrifuge and wash 3 times with 3% HCl and deionized water at 20,000 rpm, and add deionized water to obtain a uniform 1mg / ml oxide Graphene aqueous solution;

[0033] (2) Add Fe(NO 3 ) 3 Solution:

[0034] 100ul of 0.1mM Fe(NO 3 ) 3 Add the solution into the graphene oxide aqueous solution, stir and mix evenly.

[0035] (3) Reduced graphene oxide:

[0036] Add 20mgNaBH 4 , stirred and mixed evenly, and reacted for 6 hours.

[0037] (4) washing and purifying graphene:

[0038] At 10,000 rpm, they were centrifuged and washed 6 times with 2% HCl and deionized water, respectively, and vacuum-dried at 60°C to obtain graphene powder.

[0039]

Embodiment 3

[0041] (1) washing and purification:

[0042] Dissolve 1 mg of graphene oxide into 10 ml of water, ultrasonically disperse and dissolve, then centrifuge and wash 3 times with 3% HCl and deionized water at 20,000 rpm, and add deionized water to obtain a uniform 0.1 mg / ml Graphene oxide aqueous solution;

[0043] (2) Join CoSO 4 Solution:

[0044] 100ul of 0.1mM CoSO 4 Add the solution into the graphene oxide aqueous solution, stir and mix evenly.

[0045] (3) Reduced graphene oxide:

[0046] Add 2 mg NaBH 4 , stirred and mixed evenly, and reacted for 6 hours.

[0047] (4) washing and purifying graphene:

[0048] At 10,000 rpm, they were washed by centrifugation with 3% HCl and water for 6 times, and vacuum-dried at 60°C to obtain graphene powder.

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Abstract

The invention provides a method for preparing a large amount of graphene by reducing graphene oxide by a chemical reduction method at room temperature. The method comprises the following steps of: firstly, adding a metal salt solution into a graphene oxide aqueous solution; secondly, adding NaBH4, and catalyzing NaBH4 to hydrolyze and release a large quantity of hydrogen atoms with high reducibility by using reduced metal particles at the room temperature; reducing the graphene oxide with the hydrogen atoms; and finally, removing metal particles through acid washing to obtain the graphene. By the method, the graphene is prepared without use of a chemical compound such as hydrazine hydrate and derivatives thereof and the like with strong toxicity and volatility as a reducing agent, so the method has the characteristics of environment friendliness, safety and the like, and the method can be implemented under a room temperature condition, and the reaction condition is mild, so that graphene defects in the reducing process are reduced.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing graphene. Background technique [0002] Graphene is the thinnest known material, with extraordinary electrical conductivity, strength dozens of times stronger than steel, and excellent light transmission. Its appearance is expected to trigger a revolution in modern electronic technology and other fields . At present, there are many methods for preparing graphene, including mechanical separation method, orientation epitaxy method, chemical vapor deposition (CVD), chemical redox method and so on. The chemical oxidation-reduction method is to oxidize and peel the natural flake graphite in an aqueous solution, and then add a reducing agent to remove the oxidized functional groups of graphene oxide to obtain graphene. Compared with several other methods, the chemical redox method has the advantages of simple process, low cost, and large-scale ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00C01B32/184
Inventor 孙旭辉卓其奇
Owner SUZHOU UNIV
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