Method for aqueous phase synthesis of manganese-doped zinc selenide adjustable-colour fluorescent quantum dot

A technology of fluorescent quantum dots and manganese doping, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of energy loss, no adjustability of fluorescence spectrum, low quantum yield, etc., and achieve simple production equipment and low energy consumption The effect of low cost and simple process

Inactive Publication Date: 2011-01-19
DONGHUA UNIV
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Problems solved by technology

However, the doping method used in the Mn:ZnSe quantum dots synthesized by Chao Wang et al. is to first generate a MnSe crystal nucleus coated with a stabilizer, and then grow a ZnSe shell around the MnSe crystal nucleus, resulting in a Mn / Zn ion melting interface (This is the Mn ion 4 T 1 → 6 A 1 Fluorescence emission center) is very thin, the quantum yield is very low (only 2.4%), and with the increase of ZnSe shell thickness, non-radiative relaxation leads to a large amount of energy loss, so its fluorescence spectrum has little tunability

Method used

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  • Method for aqueous phase synthesis of manganese-doped zinc selenide adjustable-colour fluorescent quantum dot
  • Method for aqueous phase synthesis of manganese-doped zinc selenide adjustable-colour fluorescent quantum dot
  • Method for aqueous phase synthesis of manganese-doped zinc selenide adjustable-colour fluorescent quantum dot

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Experimental program
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Effect test

Embodiment 1

[0035] Under nitrogen protection atmosphere, 0.0247g selenium powder and 0.0299gNaHB 4 Dissolve in 10mL high-purity water to prepare NaHSe solution for later use. 1.064g MPA was dissolved in high-purity water, then the pH of the above solution was adjusted to 11.0 with 2.0mol / L NaOH solution and the volume was fixed to 10mL, and the prepared stabilizer solution was placed in a fume hood for subsequent use. 0.0495g MnCl 2 4H 2 O was dissolved in 10 mL of high-purity water to prepare Mn 2+ The solution is ready for use. 0.1372g Zn(OAc) 2 2H 2 O was dissolved in 25mL high-purity water to prepare Zn 2+ The solution is ready for use.

[0036] 1mL Mn 2+ The solution was placed in a 50mL three-necked flask, passed through nitrogen for 30min, and then heated to 100°C with an oil bath to reflux. The newly prepared NaHSe solution was quickly injected into the above solution and refluxed for 40 minutes to obtain MnSe nanocrystal nuclei; the reaction solution was cooled to 80°C, ...

Embodiment 2

[0042] Under nitrogen protective atmosphere, 0.0247g selenium powder and 0.0449gNaHB 4 Dissolve in 10mL high-purity water to prepare NaHSe solution for later use. 0.3546g MPA was dissolved in high-purity water, then the pH of the above solution was adjusted to 12.0 with 2.0mol / L NaOH solution and the volume was fixed to 10mL, and placed in a fume hood for later use. 0.0495g MnCl 2 4H 2 O was dissolved in 10 mL of high-purity water to prepare Mn 2+ The solution is ready for use. 0.2058g Zn(OAc) 2 2H 2 O was dissolved in 25mL high-purity water to prepare Zn 2+ The solution is ready for use.

[0043] 1mL Mn 2+ The solution was placed in a 50mL three-necked flask, passed through nitrogen for 30min, and then heated to 100°C with an oil bath to reflux. The newly prepared NaHSe solution was quickly injected into the above solution and refluxed for 20 minutes to obtain MnSe nano crystal nucleus. The reaction solution was cooled to 70°C, 1mL Zn(OAc) 2 Add it into the flask w...

Embodiment 3

[0045] Under nitrogen protection atmosphere, 0.0371g selenium powder and 0.0598gNaHB 4 Dissolve in 10mL high-purity water to prepare NaHSe precursor solution for later use. 1.596g MPA was dissolved in high-purity water, then the pH of the above solution was adjusted to 13.0 with 2.0mol / L NaOH solution and the volume was fixed to 10mL, and placed in a fume hood for later use. 0.0495g MnCl 2 4H 2 O was dissolved in 10 mL of high-purity water to prepare Mn 2+ The solution is ready for use. 0.2744g Zn(OAc) 2 2H 2 O was dissolved in 25mL high-purity water to prepare Zn 2+ The solution is ready for use.

[0046] 1mL Mn 2+ The precursor solution was placed in a 50mL three-necked flask, nitrogen gas was passed for 30min, and then the temperature was raised to 90°C with an oil bath to reflux. The newly prepared NaHSe solution was quickly injected into the above solution and refluxed for 60 minutes to obtain MnSe nano crystal nucleus. The reaction solution was cooled to 60°C, ...

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Abstract

The invention relates to a method for the aqueous phase synthesis of a manganese-doped zinc selenide adjustable-colour fluorescent quantum dot. Firstly, MnSe / ZnSe crystal nucleus is generated; and then, a method of stabilizer coating and the epitaxial growth of a ZnSe shell is used, the separation of crystal nucleation and growth steps is controlled to regulate the shell framework growth mode andthe reaction time, and an MnSe:ZnSe quantum dot is synthesized in the aqueous phase, thus an Mn ion 4T1-6A1 fluorescence emission center is strengthened (Mn / Zn mutual-melting interface) to increase the quantum yield to 4.8%, and the fluorescence launch emission spectrum is controlled and adjusted to 602 nm from 572 nm by prolonging the epitaxial growth time of the ZnSe shell. The invention has simple preparation technology, requires simple production equipment and is easy to realize industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of manganese-doped zinc selenide, in particular to a method for synthesizing manganese-doped zinc selenide color-tunable fluorescent quantum dots in water phase. Background technique [0002] Mn:ZnSe fluorescent quantum dots have attracted more and more attention due to their superior optical properties (quantum confinement effect), chemical stability and low toxicity, and they hope to be used in the field of bioluminescent label detection. For Mn:ZnSe quantum dots, divalent manganese ions are a stronger Lewis acid than divalent zinc ions, so it is very difficult to prepare high-performance Mn:ZnSe quantum dots by traditional methods. It was not until X.Peng et al. used the idea of ​​nucleation doping to synthesize high-performance Mn:ZnSe quantum dots on the basis of organometallic method (X.Peng, et al., J.Am.Chem.Soc.2005, 127, 17586-17587). The Mn:ZnSe quantum dots synthesized by X.Peng et al. hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/57C09K11/02
Inventor 王宏志邵澎涛李耀刚张青红
Owner DONGHUA UNIV
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