Method for preparing high-quality graphene quantum dot or large-lamella graphene oxide

A graphene quantum dot, high-quality technology, applied in the direction of graphene, single-layer graphene, chemical instruments and methods, etc., can solve the problems of complex operation and low strategy efficiency, achieve good water solubility, uniform size, and improve peeling efficiency effect

Active Publication Date: 2019-03-19
HENAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this post-processing strategy is inefficient and complicated to operate. Therefore, the preparation of graphene quantum dots with uniform size and single chemical composition by a simple method is still a difficulty in current research.

Method used

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  • Method for preparing high-quality graphene quantum dot or large-lamella graphene oxide
  • Method for preparing high-quality graphene quantum dot or large-lamella graphene oxide
  • Method for preparing high-quality graphene quantum dot or large-lamella graphene oxide

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Embodiment 1

[0029] A method for preparing graphene quantum dots, the steps are as follows:

[0030]Highly oriented and regular highly oriented pyrolytic graphite is partially coated with paraffin to expose the (002) crystal plane, which is used as an anode. Under the condition of applying a constant voltage of 3V, the electrochemical reaction was carried out in a 10 mol / L NaOH alkaline electrolyte solution to obtain graphene quantum dots dispersed in an alkaline electrolyte aqueous solution. The mixed solution of gained quantum dots and electrolyte is diluted, and the quantum dot solution is neutralized with 0.1mol / L dilute hydrochloric acid solution, and the solution is dialyzed for 3 days in a dialysis bag with a molecular weight cut-off of 3000 Da, and the salt in the solution is All removed, namely obtain the graphene quantum dot aqueous solution with uniform size distribution. The graphene quantum dot aqueous solution after dialysis is freeze-dried to obtain blue fluorescent graphen...

Embodiment 2

[0033] A method for preparing graphene oxide, the steps are as follows:

[0034] Pyrolytic graphite was partially coated with paraffin to expose the (002) crystal plane, which was used as the anode. Under the condition of external constant voltage 4V, in 0.1mol / L H 2 SO 4 The electrochemical reaction is carried out in the electrolyte solution to obtain graphene oxide dispersed in the acidic electrolyte solution. The electrolyte solution of the obtained product was vacuum filtered at 0.05MPa / 1 minute, washed with deionized water several times, and freeze-dried (freezing temperature: -50°C, drying temperature: 0°C, drying vacuum: 1Pa, drying time: 48 hours) After that, high-quality graphene oxide is obtained.

Embodiment 3

[0036] A method for preparing graphene oxide, the steps are as follows:

[0037] Highly oriented and regular highly oriented pyrolytic graphite is partially coated with paraffin to expose the (002) crystal plane, which is used as an anode. Under the condition of alternating voltage of 2V-5V, at 0.1mol / L Na 2 SO 4 The electrochemical reaction is carried out in the electrolyte solution to obtain graphene oxide dispersed in the acidic electrolyte solution. The resulting product electrolyte solution was vacuum filtered at 0.2MPa / 120 minutes, washed with deionized water several times, and freeze-dried (freezing temperature: liquid nitrogen temperature, drying temperature: 20°C, drying vacuum: 14Pa, drying time: 1 hour) After that, high-quality graphene oxide is obtained.

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Abstract

The invention provides a method for preparing a high-quality graphene quantum dot or large-lamella graphene oxide. The high-quality graphene quantum dot or large-lamella graphene oxide can be respectively prepared from highly-oriented pyrolytic graphite or pyrolytic graphite with a relatively high orientation degree, graphite foil and the like serving as raw materials by using a controllable selective crystal surface electrochemical stripping method. A single crystal surface is selected to be exposed into an electrolyte to be subjected to an electrochemical stripping reaction by utilizing a difference of electrochemical reaction energy of different crystal surfaces of graphite, and thus, large-lamella graphene oxide is obtained in an acidic or neutral electrolyte; and a blue fluorescent graphene quantum dot which is high in yield, capable of realizing further separation without aftertreatment, good in water solubility, uniform in size, unique in chemical component and narrow in spectrum and has a half-peak breadth is prepared in an alkaline electrolyte.

Description

technical field [0001] The invention relates to the technical field of preparation of graphene quantum dots, in particular to a method for preparing high-quality graphene quantum dots or large sheets of graphene oxide. Background technique [0002] Strictly speaking, graphene quantum dots refer to graphene with a lateral dimension below 20 nm and a thickness less than or equal to 3 layers. The size of graphene quantum dots is smaller than the exciton Bohr radius, which causes the movement of electrons and holes inside the atoms to be strictly restricted in all directions, so it has a very significant quantum confinement effect. As a new type of quantum dots, graphene quantum dots have both the excellent properties of graphene and quantum dots. Compared with traditional quantum dots such as CdS, CdTe, etc., graphene quantum dots have better biocompatibility and non-toxicity, which greatly expands the application range of quantum dots in organisms and cells. At the same time...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/198C09K11/65
CPCC01B32/184C01B32/198C01B2204/02C01B2204/04C01B2204/32C09K11/65
Inventor 张经纬王慧阎利卫张纪伟龚春红
Owner HENAN UNIVERSITY
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