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Method for preparing water-soluble fluorescent ZnSe/ZnS core-shell quantum dots

A water-soluble, quantum dot technology, applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of high cost and long test period, and achieve the effects of cheap price, reduced energy consumption, and simple process

Inactive Publication Date: 2010-07-28
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this preparation method requires special microwave reaction equipment, which is costly, and after the ZnSe quantum dots are prepared, it needs to be placed in an ordinary light environment for photodegradation, so as to obtain high fluorescence quantum efficiency water-soluble ZnSe / ZnS core-shell Type quantum dots, although the preparation method is simple, but the test cycle is long, it takes 1 to 30 days

Method used

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  • Method for preparing water-soluble fluorescent ZnSe/ZnS core-shell quantum dots
  • Method for preparing water-soluble fluorescent ZnSe/ZnS core-shell quantum dots
  • Method for preparing water-soluble fluorescent ZnSe/ZnS core-shell quantum dots

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Embodiment 1

[0025] The preparation method of water-soluble fluorescent ZnSe / ZnS core-shell quantum dot among the present invention, its specific steps are:

[0026] (1) prepare the NaSeH solution as the selenium source:

[0027] Take 1.5×10 -4 mol of NaBH 4 with 7.5×10 -5 mol of Se powder was placed in a 20mL three-neck flask, 5mL of distilled water was added, heated to 30°C under nitrogen protection, and reacted for 30 minutes to obtain a NaSeH solution.

[0028] (2) Preparation of ZnSe precursor solution and co-precipitation method to prepare ZnSe quantum dots

[0029] will be 6×10 -4 mol Zn(Ac) 2Dissolve in 20mL of distilled water, add 50 microliters of 90% thioglycolic acid, adjust the pH to 9.6 with 1mol / L NaOH solution, inject 5ml of NaSeH solution as the ZnSe precursor solution, and heat the obtained ZnSe precursor solution To 90 degrees Celsius, and continuous magnetic stirring, reflux, after 60 minutes, take it out and put it in the refrigerator for rapid cooling to obtain ...

Embodiment 2

[0032] The preparation method of water-soluble fluorescent ZnSe / ZnS core-shell quantum dot among the present invention, its specific steps are:

[0033] (1) prepare the NaSeH solution as the selenium source:

[0034] Take 0.003mol of NaBH 4 Put 0.001mol of Se powder into a 20mL three-neck flask, add 1mL of distilled water, heat to 40°C under nitrogen protection, and react for 45 minutes to obtain NaSeH solution;

[0035] (2) Preparation of ZnSe precursor solution and co-precipitation method to prepare ZnSe quantum dots

[0036] 0.002mol Zn(Ac) 2 Dissolve in 20mL of distilled water, add 55 microliters of thioglycolic acid with a concentration of 90%, adjust the pH=8.7 with 1mol / L NaOH solution, inject 1ml of NaSeH solution as the precursor solution of ZnSe; the obtained ZnSe precursor solution Heating to 90 degrees Celsius, and continuous magnetic stirring and reflux, after 90 minutes, take it out and put it in the refrigerator for rapid cooling to obtain water-soluble ZnSe ...

Embodiment 3

[0040] The preparation method of water-soluble fluorescent ZnSe / ZnS core-shell quantum dot among the present invention, its specific steps are:

[0041] (1) prepare the NaSeH solution as the selenium source:

[0042] Take 0.0008mol of NaBH 4 Put 0.0002mol of Se powder into a 20mL three-necked flask, add 5mL of distilled water, heat to 30 degrees Celsius under nitrogen protection, and react for 30 minutes to obtain NaSeH solution;

[0043] (2) Preparation of ZnSe precursor solution and co-precipitation method to prepare ZnSe quantum dots

[0044] 0.004mol Zn(Ac) 2 Dissolve in 20 mL of distilled water, add 60 microliters of thioglycolic acid with a concentration of 90%, adjust the pH=10 with 1 mol / L NaOH solution, inject 5 milliliters of NaSeH solution as the precursor solution of ZnSe; the obtained ZnSe precursor solution Heating to 90 degrees Celsius, and continuous magnetic stirring and reflux, after 50 minutes, take it out and put it in the refrigerator for rapid cooling ...

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Abstract

The invention belongs to the technical field of nano-material preparation techniques and biological analysis detection, and in particular relates to a method for preparing water-soluble fluorescent ZnSe / ZnS core-shell quantum dots. The method comprises: adopting a coprecipitation method and taking thioglycollic acid as surfactant to synthesize ZnSe quantum dots in aqueous solution; adding excessive Zn precursor solution to reaction solution dropwise so as to enrich a large number of Zn2+ ions on the surface of quantum dots; adding (NH4)2S solution dropwise to the solution at a certain rate and controlling temperature so as to ensure that S2- subsequently added and Zn2+ ions enriched on the surface are covalently bound to form a ZnS shell; and avoiding the uniform nucleation of ZnS by adjusting experimental parameters. The core-shell quantum dots prepared by the method are compact in core-shell structure, and the quantum dots uniform in size distribution (3 to 6 nanometers) can be obtained without further size separation.

Description

technical field [0001] The invention belongs to the technical fields of nanometer material preparation and biological analysis and detection, and in particular relates to a preparation method of water-soluble fluorescent ZnSe / ZnS core-shell quantum dots. Background technique [0002] Quantum dots are a class of semiconductor nanocrystals composed of II-VI or III-V elements whose radius is smaller than or close to the exciton Bohr radius, also known as semiconductor nanocrystals. Quantum dots have a quantum size effect, and their optical properties change with particle size, and their luminous efficiency is also greatly improved compared with bulk materials. In 1998, Alivisatos and Nie SM first reported the use of semiconductor nanocrystals instead of organic fluorescent dyes as biomolecular markers, and successfully labeled transferrin and immunoglobulin (Alivisatos.et, Science, 1998, 281, 2013~ 2016; Nie SM.et, science, 1998, 281, 2016-2018), predicting the great applicati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88
Inventor 刘福田陈秀秀孙莉杨萍姜庆辉张爱玉
Owner UNIV OF JINAN
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