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Preparation method of ZnSe/ZnS core-shell quantum dots

A core-shell structure, quantum dot technology, applied in the synthesis field of fluorescent nanomaterials, can solve the problems of complex operation process, high condition requirements, ZnSe quantum dots do not have hydrophilicity, etc., to simplify the synthesis process, overcome the complex process, The effect of saving reaction time

Inactive Publication Date: 2012-06-27
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ZnSe quantum dots synthesized in the organic phase are not hydrophilic, and must be exchanged into the water phase through ligand exchange before being applied to the biological system. The operation process is complicated and the conditions are high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Below by embodiment, further illustrate outstanding feature of the present invention, only in order to illustrate the present invention and in no way limit the present invention.

[0023] A ZnSe / ZnS core-shell quantum dot, which consists of: selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 O), thioglycolic acid (TGA), and the rest are aqueous solutions.

[0024] In the described ZnSe / ZnS core-shell structure quantum dots, selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 O), the molar ratio of thioglycolic acid (TGA) is 1 / 10:1:2.4 respectively, and the ultraviolet lamp (254nm) of 30W is irradiated for 20-60h.

[0025] The pH value of the solution is 12.

[0026] A kind of illumination-assisted room temperature preparation method of ZnSe / ZnS core-shell structure quantum dots, its steps are:

[0027] 1. Prepare potassium selenium hydride solution by reducing selenium powder with potassium borohydride: weigh 0.3000g potassium borohydride and 0.1184g selenium powder r...

Embodiment 2

[0035] A ZnSe / ZnS core-shell quantum dot, which consists of: selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 O), thioglycolic acid (TGA), and the rest are aqueous solutions.

[0036] In the described ZnSe / ZnS core-shell structure quantum dots, selenium powder (Se), zinc acetate (Zn(Ac) 2 2H 2 The molar ratios of O) and thioglycolic acid (TGA) were 1 / 5:1:2.4, respectively, and irradiated with a 30W ultraviolet lamp (254nm) for 48h.

[0037] The pH value of the solution is 13.

[0038] A method for preparing ZnSe / ZnS core-shell structure quantum dots at room temperature (20-25°C, the same below) under illumination, the steps of which are:

[0039] 1. Prepare potassium selenium hydride solution by reducing selenium powder with potassium borohydride: weigh 0.5000g potassium borohydride and 0.1974g selenium powder respectively in a test tube with a soft stopper, add 10mL deionized water to it, plug the stopper, and React in an ice bath for 2.5 hours to obtain a colorless and...

Embodiment 3

[0046] A kind of illumination-assisted room temperature preparation method of ZnSe / ZnS core-shell structure quantum dots, its steps are:

[0047] 1. Weigh 0.5000g of potassium borohydride and 0.1974g of selenium powder into a test tube with a soft stopper, add 5mL of deionized water to it, put the stopper on, and react in an ice bath for 3 hours to obtain a colorless transparent liquid of 0.50 The potassium selenide solution of mol / L;

[0048] 2. Weigh another 1.0975g Zn(Ac) 2 2H 2 O crystals were dissolved in 200mL deionized water to obtain a 0.025mol / L zinc acetate solution;

[0049] 3. Pipette 0.69mL of thioglycolic acid into the zinc acetate solution, and adjust the pH value to 14 with 5mol / L sodium hydroxide solution;

[0050] 4. Adjust the zinc acetate solution with a pH value of 14 to pass nitrogen for half an hour to remove dissolved oxygen, quickly add 2mL of 0.50mol / L potassium selenium hydride solution, and continue to pass nitrogen for 45-30min to make it fully ...

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Abstract

The invention discloses a preparation method of ZnSe / ZnS core-shell quantum dots through illumination assisted room-temperature synthesis. The method comprises the steps of: A. preparing a potassium hydrogen selenide solution by reducing selenium powder with potassium borohydride; B. weighing zinc acetate crystals, which is then dissolved in deionized water to a constant volume, thus obtaining a zinc acetate solution; C. adding quantitative thioglycolic acid into the zinc acetate solution; D. adjusting the solution to a specific pH value with a sodium hydroxide solution; E. after introducing an inert gas for deoxygenation, adding the potassium hydrogen selenide solution; F. placing the stock solution or a diluted solution of the mixed solution under an ultraviolet light for radiation for a certain period of time, and conducting detection with fluorescence spectrum analysis; and G. adding isopropyl alcohol for purification, then carrying out drying by a freeze drier so as to obtain ZnSe / ZnS core-shell quantum dot solid powder, which is dissolved in a PBS solution or deionized water before using, thus obtaining a ZnSe / ZnS core-shell quantum dot solution. The method of the invention has the advantages of simple process, easily controllable technological parameters, as well as cheap raw materials. The synthesized ZnSe / ZnS core-shell quantum dots are free of heavy metal ions, and can be used for biological labeling and imaging.

Description

technical field [0001] The invention relates to the synthesis of fluorescent nanomaterials, and more specifically to a method for preparing ZnSe / ZnS core-shell quantum dots at room temperature in aqueous phase. The synthesized quantum dots do not contain heavy gold ions and can be used for biomarking and imaging. Background technique [0002] ZnSe quantum dots have become a research hotspot because they do not contain heavy metal ions and have high biocompatibility. The ZnSe quantum dots synthesized in the organic phase are not hydrophilic, and must be exchanged into the water phase through ligand exchange before being applied to the biological system. The operation process is complicated and the conditions are high. Quantum dots prepared by aqueous phase synthesis can be directly used in biological probes, and its research has attracted more and more attention, and the research on this aspect has progressed rapidly. Among them, the most studied one is the hydrothermal synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/88
Inventor 周培疆詹红菊丁玲何振宇
Owner WUHAN UNIV
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