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A method for large-scale preparation of highly efficient red/near-infrared emitting fluorescent carbon dots

A technology for large-scale preparation of fluorescent carbon dots, applied in luminescent materials, chemical instruments and methods, nano-optics, etc., can solve the problems of low efficiency of red carbon dots, poor environmental stability, unfavorable technical applications, etc. The effect of production, low cost, simple and convenient reaction

Active Publication Date: 2021-07-20
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still large questions regarding the efficient synthesis of fluorescent carbon dots with infrared and near-infrared emission
[0004] The maximum emission wavelength of the reported red fluorescent carbon dots does not exceed 760nm, and most of the fluorescence efficiency is very low, and the fluorescence intensity is weak, which greatly limits the application of carbon dots in the field of luminescence and biological imaging.
At present, there are few reports on high-efficiency red fluorescent carbon dots. Most of the synthesized carbon dots are almost synthesized in the liquid phase environment, and need to be further purified. The process is very cumbersome and the production cost is relatively high. In order to synthesize efficient red fluorescent carbon dots The researchers used the solvothermal method to control the formation of sp2 domains or modify the surface functional groups of carbon dots to conduct experiments. The efficiency of red carbon dots synthesized by this method is often not high, the environmental stability is poor, and it is difficult to store for a long time, which is not conducive to further research. technology application

Method used

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  • A method for large-scale preparation of highly efficient red/near-infrared emitting fluorescent carbon dots
  • A method for large-scale preparation of highly efficient red/near-infrared emitting fluorescent carbon dots
  • A method for large-scale preparation of highly efficient red/near-infrared emitting fluorescent carbon dots

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Effect test

Embodiment 1

[0030] A method for large-scale preparation of high-efficiency red / near-infrared emitting fluorescent carbon dots, which is prepared from o-phenylenediamine and inorganic metal salts or o-phenylenediamine and dilute hydrochloric acid. The inorganic metal salt in the present invention may also be a crystalline inorganic metal salt.

[0031] The method for large-scale preparation of high-efficiency red / near-infrared emitting fluorescent carbon dots, the specific steps are: grinding o-phenylenediamine and inorganic metal salt into a powder with uniform particles, mixing the two evenly to obtain a mixed powder; mixing The powder is transferred to the lining of the reaction kettle, then packaged, transferred to the drying box, and the reaction temperature and reaction time are set. After the reaction is complete, the temperature of the drying box is cooled to room temperature, and the reaction kettle is taken out to obtain the product; the product is transferred to Wash the product...

Embodiment 2

[0042] Grind 1.62g of o-phenylenediamine and 0.23g of crystalline aluminum chloride into a powder with uniform particles, transfer the mixed powder to the lining of a 50ml reactor, then package it, transfer it to a dry box, set the reaction temperature to 200°C and The reaction time is 12 hours. After the reaction is complete, the temperature of the drying oven is cooled to room temperature, and the product is taken out; the product is transferred to a 200ml glass cup, and the product is washed with deionized water to remove unreacted precursors and certain impurities, and then After drying, high-purity red carbon dot solid powder can be obtained. The product was weighed, and 1.57g carbon dots were obtained in this embodiment, and the yield reached 85%.

[0043] The above products were tested by transmission electron microscopy, red fluorescence, near-infrared fluorescence, four-photon fluorescence, and environmental stability spectra. The results are as follows: Figure 1~6 ...

Embodiment 3

[0045] Grind 1.15g of o-phenylenediamine and 0.23g of crystalline aluminum chloride into a powder with uniform particles, transfer the mixed powder to the lining of a 50ml reactor, then package it, transfer it to a dry box, set the reaction temperature to 180°C and The reaction time is 10 hours. After the reaction is complete, the temperature of the drying box is cooled to room temperature, and the reaction kettle is taken out to obtain the product; the product is transferred to a 200ml glass cup, and the product is washed with deionized water to remove unreacted precursors and certain impurities, and then dried to obtain high-purity red carbon dot solid powder. The product was weighed, and 1.15 g of carbon dots were obtained in this embodiment, and the yield reached 83%.

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Abstract

The invention discloses a method for large-scale preparation of high-efficiency red / near-infrared emitting fluorescent carbon dots, that is, o-phenylenediamine and inorganic metal salts are ground into powders with uniform particles, and the mixed powder of o-phenylenediamine and inorganic metal salts or o-phenylenediamine The mixture of phenylenediamine and dilute hydrochloric acid is transferred to the inner lining of the reaction kettle, then packaged, transferred to the drying box, and the reaction temperature and reaction time are set. After the reaction is complete, the temperature of the drying box is cooled to room temperature, and the reaction kettle is taken out. The product is obtained; the product is washed and dried. Compared with the prior art, the reaction of the present invention is simple and convenient, without purification, low cost, convenient for large-scale production, good environmental stability, convenient storage and transportation, and the prepared fluorescent carbon dots have excellent red fluorescence performance, and have four-photon Fluorescent properties, and for the first time realized the fluorescence emission of carbon dots in the third near-infrared window; carbon dot products can meet the production requirements of various optoelectronic devices without complicated modification in the later stage.

Description

technical field [0001] The invention belongs to the technical field of fluorescent carbon dot preparation methods, and in particular relates to a method for large-scale preparation of highly efficient red / near-infrared emitting fluorescent carbon dots. Background technique [0002] Nowadays, nanomaterials have gradually entered various fields of our lives. A variety of carbon-based fluorescent nanomaterials, such as carbon nanodots, fluorescent carbon nanotubes, polymer dots, graphene quantum dots, and nanodiamonds, have been synthesized and applied. Carbon nanomaterials have attracted extensive research by scientists because of their great potential in various technological applications. The excellent electronic and physical and chemical properties of carbon dots have made their optical properties attract great attention from researchers in recent years. [0003] As an emerging fluorescent nanomaterial, carbon dots have great application potential in the fields of chemica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/65B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/65
Inventor 宋世玉刘凯凯单崇新
Owner ZHENGZHOU UNIV
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