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A method for preparing graphene quantum dots based on ozone oxidation

A graphene quantum dot, ozone oxidation technology, applied in graphene, nanotechnology for materials and surface science, nanocarbon, etc., can solve the time consumption (some require more than 10 days of preparation, limit large-scale preparation and application, the difficulty of separation of graphene quantum dots, etc., to achieve the effect of good fluorescence and electrochemical catalytic activity, rich oxygen-containing groups, and mild conditions

Active Publication Date: 2018-12-04
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, harsh reaction conditions (such as high temperature), time consumption (some require more than 10 days of preparation), low yield and damage to the aromatic carbon skeleton limit its large-scale preparation and application.
[0004] Literature (Photo-Fenton reaction of graphene oxide:A new strategy toprepare graphene quantum dots for DNA cleavage.Acs Nano 6.8(2012):6592-6599) reports a method for preparing graphene quantum dots by using the Fenton method to oxidize GO, This method is simple and convenient, but the addition of iron ions will make the separation of extremely small graphene quantum dots extremely difficult

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  • A method for preparing graphene quantum dots based on ozone oxidation
  • A method for preparing graphene quantum dots based on ozone oxidation
  • A method for preparing graphene quantum dots based on ozone oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A method for preparing graphene quantum dots, comprising the steps of:

[0045] 1) Use the Brodie method to prepare graphite oxide; dilute the graphene oxide aqueous solution from 0.5mg / mL to 0.25mg / mL as the stock solution, add 10mL stock solution and 10mL ultrapure water to the sample bottle, a total of 20mL, to obtain a concentration of 0.125mg / mL The aqueous dispersion of graphite oxide in mL;

[0046] 2) Adjust the ozone generator to stabilize the ozone concentration at 50g / m 3 ;Put the sample bottle in an ultrasonic cleaner at 25°C, pass through ozone, and react for 60 minutes; after the ozone is stopped, take out the sample bottle and blow it with nitrogen for 10 minutes.

[0047] 3) The reaction solution was divided into 5mL or 10mL pipettes, and subjected to vacuum freeze-drying.

[0048] Through fluorescence spectrum scanning, infrared spectrum and ultraviolet spectrum analysis, it is known that the graphene quantum dots obtained in this example have a maxim...

Embodiment 2

[0050] A method for preparing graphene quantum dots, comprising the steps of:

[0051] 1) Use the Hummers method to prepare graphite oxide; dilute the graphene oxide aqueous solution from 0.5mg / mL to 0.25mg / mL as the stock solution, add 10mL stock solution and 10mL ultrapure water to the sample bottle, a total of 20mL, to obtain a concentration of 0.125mg / mL The aqueous dispersion of graphite oxide in mL;

[0052] 2) Add 1 mL of H 2 o 2 .

[0053] 3) Adjust the ozone generator to stabilize the ozone concentration at 50g / m 3 ;Put the sample bottle in an ultrasonic cleaner at 25°C, pass in ozone, and react for 180 minutes; after the ozone is stopped, take out the sample bottle and blow it with nitrogen for 10 minutes.

[0054] 4) The reaction solution was divided into 5mL or 10mL pipettes, and subjected to vacuum freeze-drying.

[0055] figure 1 It is the scanning electron microscope picture of the graphene quantum dot gained in embodiment 2; figure 2 It is a partially e...

Embodiment 3

[0058] A method for preparing graphene quantum dots, comprising the steps of:

[0059] 1) Use the Hummers method to prepare graphite oxide; disperse it in water to form 20 mL of an aqueous dispersion with a concentration of 10 mg / mL by ultrasonic exfoliation;

[0060] 3) Adjust the ozone generator to stabilize the ozone concentration at 30g / m 3 ;Put the sample bottle in an ultrasonic cleaner at 10°C, pass through ozone, use ultraviolet radiation, and react for 120 minutes; after the ozone is stopped, take out the sample bottle and blow it with nitrogen for 10 minutes, and the nitrogen flow rate can continuously blow out bubbles of normal size appropriate;

[0061] 4) The reaction solution was divided into 5mL or 10mL pipettes, and subjected to vacuum freeze-drying.

[0062] Through fluorescence spectrum scanning, infrared spectrum and ultraviolet spectrum analysis, it is known that the graphene quantum dots obtained in this example have a maximum emission spectrum at 530 nm ...

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Abstract

The invention relates to an ozonation-based method for preparing graphene quantum dots. By using oxidized graphene as a raw material, large size oxidized graphene is cut to finally obtain a graphene quantum dot product by adopting a method based on ozone or an advanced oxidization method based on coupled oxidization of ozone or one or two of ozone, hydrogen peroxide, ultraviolet rays and ultrasound. As an oxidization method of ozone or a co-oxidation method of or ozone, hydrogen peroxide, ultraviolet rays The method provided by the invention is adopted, compared with a conventional preparation method, the method provided by the invention has the characteristics of being mild in condition and fast to react, and is free of needs of adding other hardly separated substances and the like. The method is a novel method for volume production of the graphene quantum dots with a broad application prospect. The material prepared by the method has rich oxygen-containing groups, relatively good fluorescence and electrochemical catalytic activity, and can be widely applied to preparing solar batteries, electrochemical biosensors, photocatalytic materials, bioimaging and the like.

Description

technical field [0001] The invention relates to a method for preparing graphene quantum dots, which belongs to the field of nanomaterial preparation, and in particular to a method for mass-producing graphene quantum dots based on an advanced ozone oxidation method for treating graphite oxide. Background technique [0002] Graphene Quantum Dots (GQDs) refer to the thickness of 1-3 graphene layers in the vertical direction, and the lateral dimension is below 100 nanometers, and the appearance is just like a very small point. GQDs have discrete electronic bands and exhibit typical semiconducting properties and are promising in many fields, such as optoelectronic devices and optoelectronic systems. In addition, its photoluminescence, ultra-small size, and nontoxicity make GQDs more suitable for cell imaging, drug delivery, and other in vitro or biological systems. Due to the fact that GQDs have more oxygen-containing groups and defects, their use as sensing electrode materials ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184B82Y30/00
Inventor 刘晨明温嘉玮李明杰曹宏斌张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI