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Preparation method for fluorescence carbon-based quantum dot

A carbon-based quantum dot and fluorescence technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of difficulty in expanding production, low yield, low yield, etc., and achieve the effect of improving quantum yield and high yield

Inactive Publication Date: 2014-03-19
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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Problems solved by technology

However, the fluorescence emission spectra of these carbon-based quantum dots are mainly in the yellow-green band, and the quantum yield is generally lower than 15%.
This limits the application of these carbon-based quantum dots in biological applications and optoelectronic materials
[0003] In recent years, a lot of work has been done on the spectrum regulation of carbon-based quantum dots at home and abroad. In terms of graphene quantum dots, the method is mainly to control the oxidation degree of graphene quantum dots. In 2013, Chem.Comm. published Near infra-red photoluminescent graphene nanoparticles greatly expand their use in noninvasive biomedical imaging, etc. used a mixture of sulfuric acid and nitric acid to oxidize and shear graphene to obtain near-infrared graphene oxide quantum dots, but the preparation method is more dangerous and Complex process, low yield, low quantum yield, difficult to repeat and mass production
[0004] On the other hand, doping carbon quantum dots can also tune its fluorescence spectrum, Hydrothermal Treatment of Grass: A Low-Cost, Green Route to Nitrogen-Doped, Carbon-Rich, Photoluminescent published in 2012 by Adv.Mater. Polymer Nanodots as an Effective Fluorescent Sensing Platform for Label-Free Detection of Cu(II)Ions, use concentrated nitric acid to reflow carbon quantum dots for a long time, and obtain N-doped carbon quantum dots with blue fluorescence, but this method The amount of doping cannot be controlled, and the luminous efficiency of the obtained carbon quantum dots is low, and the preparation is complicated, the yield is low, and the experiment is not easy to repeat and mass production
In addition, this method cannot be applied to doping carbon quantum dots or other carbon-based quantum dots with other elements.
In addition, the existing spectrum control methods of graphene quantum dots and carbon quantum dots cannot be used universally, and there are difficulties in expanding production

Method used

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  • Preparation method for fluorescence carbon-based quantum dot
  • Preparation method for fluorescence carbon-based quantum dot
  • Preparation method for fluorescence carbon-based quantum dot

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preparation example Construction

[0060] Such as figure 1 As shown, the preparation method of the fluorescent carbon-based quantum dots at least includes:

[0061] First, step S10 is performed: providing oxidized carbon-based quantum dot powder;

[0062] Wherein, the oxidized carbon-based quantum dot powder in this step can also be directly produced by carbon materials, specifically, combined with figure 1 ,refer to figure 2 Shown, the preparation method of the carbon-based quantum dot powder of described oxidation comprises:

[0063] Step S11: providing carbon material;

[0064] In this step, there is no specific requirement for the carbon material, and generally amorphous carbon, carbon black, graphene, graphene oxide, graphene nanosheets, fullerene, mesoporous carbon, or graphite can be used. Preferably, the carbon material is graphite, carbon black, graphene, graphene oxide, graphene nanosheets, fullerenes, mesoporous carbon or carbon nanotubes.

[0065] Step S12: adding a mixed solution of nitric ...

Embodiment 1

[0109] combine figure 1 and figure 2 , first, perform step S10: provide oxidized carbon quantum powder;

[0110] Specifically, in this embodiment, in this step, an oxidized carbon-based quantum powder is provided, including:

[0111] Step S11: Provide 25.000g of carbon black powder (particle size 20-50nm);

[0112] Step S12: Add the carbon black powder into a mixture of 285mL concentrated nitric acid (concentration: 67wt%) and 535mL concentrated sulfuric acid (concentration: 98wt%), mechanically stir at 5°C for 30min, and the stirring rate is 600r / min to form the first a mixed liquid;

[0113] Step S13: Slowly add 300g of NaClO to the first mixed liquid 3 In order to generate an oxidation reaction, control the reaction temperature of the oxidation reaction to 0-10°C, and react for 5 hours to form a second mixed liquid;

[0114] Step S14: Cool the second mixed liquid to room temperature, add 500 mL of distilled water to dilute to form a third mixed liquid, and filter it ...

Embodiment 2

[0126] Change the carbon black in Example 1 to 25.000g graphene powder (1 to 5 atomic layers, the lateral dimension is 200-500nm), the dopant is changed to 0.050mL boron trifluoride ether solution, and other conditions are not changed. Change, B, F doped graphene quantum dots with an emission wavelength of 450nm can be obtained. This material can produce strong green fluorescence under ultraviolet light irradiation, with a quantum yield of 0.37.

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Abstract

The invention provides a preparation method for a fluorescence carbon-based quantum dot. The preparation method for the fluorescence carbon-based quantum dot at least comprises the steps of providing oxidized carbon-based quantum dot powder; providing a solvent, and dispersing the oxidized carbon-based quantum dot powder into the solvent to obtain the oxidized carbon-based quantum dot solution; adding a doping agent into the oxidized carbon-based quantum dot solution, reducing the oxidized carbon-based quantum dot by utilizing the solvent thermal reaction so as to obtain the doped carbon-based quantum dot. According to the invention, the technical scheme that oxidized carbon-based quantum dot is taken as a raw material and the solvent thermal reduction and doping are synchronously carried out is adopted, the carbon-based quantum dot represented by graphene quantum dot and carbon quantum dot can be reduced and doped by adopting various easily available nonmetal compounds or metal compounds through the solvent thermal reaction, the yield of a product is high, the regulation on the fluorescent spectrum of the carbon-based quantum dot can be realized, and the yield of quantum can be improved.

Description

technical field [0001] The invention relates to the field of new inorganic materials, in particular to a method for preparing fluorescent carbon-based quantum dots. Background technique [0002] Carbon-based quantum dots, represented by graphene quantum dots and carbon quantum dots, are used in up-conversion optoelectronic materials and fluorescent labeling due to their excellent luminescent properties, low cytotoxicity, good water solubility, stable fluorescence and excellent biocompatibility. , fluorescent coatings, fluorescent probes, and photodynamic therapy have broad application prospects and have received extensive attention. However, the fluorescence emission spectra of these carbon-based quantum dots are mainly in the yellow-green band, and the quantum yield is generally lower than 15%. This limits the application of these carbon-based quantum dots in biological applications and optoelectronic materials. [0003] In recent years, a lot of work has been done on the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/65C09K11/87C09K11/88
Inventor 杨思维孙静李修兵丁古巧谢晓明江绵恒
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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