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Method of ultrasonic combining microwave for preparing graphene quantum dots

A technology of graphene quantum dots and ultrasonic waves, applied in graphene, chemical instruments and methods, carbon compounds, etc., can solve problems such as difficult operation, harsh preparation conditions, and complicated steps, and achieve less edge defects, simple process, and high yield high effect

Inactive Publication Date: 2018-05-15
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are still many problems to be overcome in the method of preparing graphene quantum dots with high reaction yield, high performance and high quality: the top-down method steps are relatively simple and the reaction yield is high, but it cannot realize the The precise control of the surface morphology and lateral dimensions of graphene quantum dots; most bottom-up methods have stronger controllability, but usually have the disadvantages of complicated steps and difficult operation; other special methods (such as electron beam etching ) mostly require harsh preparation conditions or dangerous operation, which limits the application and promotion of these methods

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  • Method of ultrasonic combining microwave for preparing graphene quantum dots
  • Method of ultrasonic combining microwave for preparing graphene quantum dots
  • Method of ultrasonic combining microwave for preparing graphene quantum dots

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Dissolve 100mg NaOH in 100ml N-methylpyrrolidone, then add 100mg graphite, stir to disperse the graphite evenly, and obtain a mixed solution;

[0042] (2) Then the mixed solution is placed in an ultrasonic cleaner, and the ultrasonic emission power is adjusted to 400W, and the ultrasonic time is 8h; then the resulting solution is placed in an ultrasonic cell disruptor, and the ultrasonic emission power is adjusted to be 360W, and the ultrasonic time is 4h; Microwave radiation heating, microwave radiation power is 600W, radiation temperature is 100℃, heating for 1h;

[0043] (3) After the reaction, the obtained reaction solution was dialyzed with distilled water for 7 days using a 500 Da dialysis bag, filtered and concentrated to 400 μg / ml by rotary evaporation to obtain graphene quantum dots.

[0044] The atomic force microscope (AFM) image of the prepared graphene quantum dots is shown in Figure 1a shown, along the Figure 1a The height profile of the middle white...

Embodiment 2

[0049] (1) Dissolve 10 mg of NaOH in 90 ml of N-methylpyrrolidone, then add 100 mg of graphite, stir to disperse the graphite evenly, and obtain a mixed solution;

[0050] (2) Then the mixed solution is placed in an ultrasonic cleaner, and the ultrasonic emission power is adjusted to 160W, and the ultrasonic time is 6h; then the resulting solution is placed in an ultrasonic cell disruptor, and the ultrasonic emission power is adjusted to be 300W, and the ultrasonic time is 2h; Microwave radiation heating, microwave radiation power is 700W, radiation temperature is 110°C, heating for 0.1h;

[0051] (3) After the reaction, the resulting reaction solution was dialyzed with distilled water for 7 days using a 500 Da dialysis bag, filtered and concentrated to 450 μg / ml by rotary evaporation to obtain graphene quantum dots.

[0052] The particle size of the prepared graphene quantum dot is 1-4nm.

[0053] N-methylpyrrolidone also has fluorescence, and its fluorescence spectrum is sh...

Embodiment 3

[0057] (1) Dissolve 50mg NaOH in 80ml N-methylpyrrolidone, then add 1000mg graphite, stir to disperse the graphite evenly, and obtain a mixed solution;

[0058] (2) Then the mixed solution is placed in an ultrasonic cleaner, and the ultrasonic emission power is adjusted to 280W, and the ultrasonic time is 4h; then the resulting solution is placed in an ultrasonic cell disruptor, and the ultrasonic emission power is adjusted to be 240W, and the ultrasonic time is 0.5h; finally Heating by microwave radiation, the microwave radiation power is 800W, the radiation temperature is 110°C, and the heating time is 0.1h;

[0059] (3) After the reaction, the obtained reaction solution was dialyzed with distilled water for 5 days using a 1000 Da dialysis bag, filtered and concentrated to 500 μg / ml by rotary evaporation to obtain graphene quantum dots.

[0060] The particle size of the prepared graphene quantum dot is 4-7nm.

[0061] The fluorescence spectrum of the prepared graphene quant...

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Abstract

The invention discloses a method of ultrasonic combining microwave for preparing graphene quantum dots. The method includes steps of: adding graphite and NaOH to N-methylpyrrolidinone, and successively performing ultrasonic stripping, crushing and microwave irradiation heating to obtain the graphene quantum dots having uniform size. In the method, with the graphite as raw material, the graphene quantum dots are prepared through ultrasonic wave and microwave in the NaOH / N-methylpyrrolidinone, so that usage of strong acid and strong oxidants is avoided. The graphene quantum dots have less edge defects and have important researching and application value in the fields of biology, medical and the like. Meanwhile, the method has simple processes and low consumption and is high in yield, whereinthe N-methylpyrrolidinone, as a dispersant of graphite, can be recycled. The method supplies a new way for synthesis of the graphene quantum dots and is beneficial to industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of preparing graphene quantum dots, in particular to a method for preparing graphene quantum dots by combining ultrasound and microwave. technical background [0002] Graphene quantum dots are a new type of quasi-zero-dimensional carbon nanomaterials based on graphene, which have stronger quantum effects and field effects than graphene. In addition, it also has low biological toxicity, excellent molecular regularity, good fluorescence effect and other properties, so it has good application potential and application prospects in nanomaterials, photoelectric materials, bioimaging, drug carriers, etc. [0003] The main synthesis method of graphene quantum dots is the top-down method, which refers to the method of using macromolecular carbon polymers such as carbon nanotubes, carbon nanofibers, graphene oxide, and graphene as carbon sources, by breaking macromolecules into Quantum-level small nanomolecules, inc...

Claims

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Application Information

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IPC IPC(8): C01B32/19B82Y40/00
CPCB82Y40/00C01B2204/32C01P2004/01C01P2004/04
Inventor 王小英蔡济海孙润仓李晓云
Owner SOUTH CHINA UNIV OF TECH
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