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Method for continuously preparing quantum dots through microchannel reactor

A technology of microchannel reactor and quantum dots, which is applied in the fields of chemical instruments and methods, nanotechnology, nano-optics, etc., can solve the problem that the continuous production of core-shell quantum dots cannot be realized, the CdSe quantum dot method needs to be improved, and the CdSe quantum dot Monodispersity is not high, to achieve the effects of industrial production, convenient production, and simple operation

Active Publication Date: 2016-06-15
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing methods, whether it is a one-pot method or a microchannel synthesis method, the synthesis of CdSe quantum dots often completes the crystal nucleation and growth process under the same conditions, which leads to low monodispersity of CdSe quantum dots and poor fluorescence spectrum. The half maximum width is above 40nm
Therefore, the method for preparing CdSe quantum dots needs to be improved
[0004] In addition, because CdSe, CdS, and CdTe quantum dots have certain biological toxicity, and the surface is easily oxidized to cause light quenching, it is often necessary to prepare core-shell quantum dots by wrapping the shell layer. The existing methods for preparing core-shell quantum dots are also often It is prepared by a one-pot method, but this method cannot realize the continuous production of core-shell quantum dots

Method used

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  • Method for continuously preparing quantum dots through microchannel reactor
  • Method for continuously preparing quantum dots through microchannel reactor
  • Method for continuously preparing quantum dots through microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) After weighing 0.0107g cadmium oxide (CdO) and 7.2228g oleylamine (OLA) in a beaker and mixing them, add 0.2mL oleic acid (OA) into the beaker, and then use 1-octadecene (ODE) to dissolve and dilute to 30mL; heat the beaker at 150°C for 1 hour to obtain a brownish-yellow transparent liquid, which is the cadmium precursor solution.

[0039] (2) Weigh 0.3948g of selenium powder (Se) in a beaker and add 4.5mL of trioctylphosphine (TOP), then dissolve and dilute to 30mL with 1-octadecene (ODE); heat the beaker at 90°C for 15min to obtain It is a colorless transparent liquid, which is the selenium precursor solution.

[0040] (3) 25 mL of the cadmium precursor solution and 25 mL of the selenium precursor solution were extracted with a syringe, and fed to the micromixer 1 through a polytetrafluoroethylene micropipe at 200 μL / min with a syringe pump.

[0041] (4) Import the cadmium precursor solution and the selenium precursor solution into the oil bath 1, and carry out t...

Embodiment 2

[0050] (1) After weighing 0.0107g cadmium oxide (CdO) and 7.2228g oleylamine (OLA) in a beaker and mixing them, add 0.2mL oleic acid (OA) into the beaker, and then use 1-octadecene (ODE) to dissolve and dilute to 30mL; heat the beaker at 150°C for 1 hour to obtain a brownish-yellow transparent liquid, which is the cadmium precursor solution.

[0051] (2) Weigh 0.3948g of selenium powder (Se) in a beaker and add 4.5mL of trioctylphosphine (TOP), then dissolve and dilute to 30mL with 1-octadecene (ODE); heat the beaker at 90°C for 15min to obtain It is a colorless transparent liquid, which is the selenium precursor solution.

[0052] (3) 25 mL of the cadmium precursor solution and 25 mL of the selenium precursor solution were extracted with a syringe, and fed to the micromixer 1 through a polytetrafluoroethylene micropipe at 200 μL / min with a syringe pump.

[0053] (4) Lead the cadmium precursor solution and the selenium precursor solution into the oil bath 1, and carry out the...

Embodiment 3

[0058] (1) Weigh 0.0107g of cadmium oxide (CdO) and 7.2228g of oleylamine (OLA) in a beaker and mix them, then add 0.2mL of oleic acid (OA) into the beaker and mix, and then dissolve and dilute with 1-octadecene (ODE) to 30 mL; heat the beaker at 150°C for 1 hour to obtain a brownish-yellow transparent liquid, which is the cadmium precursor solution.

[0059] (2) Weigh 0.3948g selenium powder (Se) with a beaker and add 4.5mL trioctylphosphine (TOP) into the beaker and mix it, then use 1-octadecene (ODE) to dissolve and dilute to 30mL; put the beaker at 90 After heating at ℃ for 15 min, a colorless transparent liquid was obtained, which was the selenium precursor solution.

[0060] (3) Weigh 0.1056g zinc diethyldithiocarbamate (ZDC) with a beaker and add 1mL trioctylphosphine (TOP) to the beaker and mix, then add 1mL oleylamine (OLA) to the beaker and mix, then Use 1-octadecene (ODE) to dissolve and dilute to 20 mL; heat the beaker at 60°C for 15 minutes to obtain a colorless ...

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Abstract

The invention discloses a method for continuously preparing quantum dots through a microchannel reactor and belongs to the field of chemical engineering. The quantum dots are cadmium selenide mononuclear quantum dots or cadmium selenide / zinc sulfide nuclear shell type quantum dots. The method comprises the steps of heating a prepared cadmium precursor solution and a selenium precursor solution to the reaction temperature, then mixing the solutions, and conducting a reaction, so that a solution of cadmium selenide quantum dots small in grain size is obtained; continuously adding the cadmium precursor solution, and making the cadmium selenide quantum dots small in grain size grow, so that a solution of cadmium selenide quantum dots large in grain size is obtained; or mixing the solution of the cadmium selenide quantum dots small in grain size with a prepared zinc sulfide precursor solution at the room temperature, and then heating the mixture to the reaction temperature for a reaction, so that a cadmium selenide / zinc sulfide nuclear shell type quantum dot solution is obtained; then conducting post-treatment on the quantum dot solution, so that the cadmium selenide nononuclear quantum dots or cadmium selenide / zinc sulfide nuclear shell type quantum dots are finally obtained. The preparation method is simple in operation and accurate to regulate, continuous production can be conducted, and the method is beneficial to industrialized production of the quantum dots.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for continuously preparing quantum dots in a microchannel reactor. Background technique [0002] Compared with traditional organic fluorescent materials, quantum dots are easily excited, emit monochromatic fluorescence, and are not easy to be photobleached. Therefore, quantum dots have a wide range of potential applications in many fields such as solar cells, light-emitting diodes, and medical treatment. Among them, group II-VI quantum dots such as CdSe, CdS, and CdTe have attracted much attention because their emitted fluorescence wavelengths can cover the entire visible spectrum. [0003] The traditional synthesis of CdSe quantum dots is a one-pot method using organic thermal solvents. Due to the factors such as temperature inhomogeneity, inability to continuously produce, and difficulty in device scale-up in the one-pot process, the production cost of qua...

Claims

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Application Information

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IPC IPC(8): C09K11/88B82Y20/00B82Y40/00C01B19/04
CPCB82Y20/00B82Y40/00C01B19/007C01P2002/80C01P2004/04C01P2006/60C09K11/883
Inventor 徐建鸿田震昊王玉军骆广生
Owner TSINGHUA UNIV
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