Microwave preparation method of water soluble ZnSe quantum dots

A quantum dot, water-soluble technology, applied in chemical instruments and methods, solution from liquid solvent at room temperature, single crystal growth, etc., can solve the problems of low fluorescence quantum efficiency and difficult preparation

Inactive Publication Date: 2010-09-15
苏州市长三角系统生物交叉科学研究院有限公司
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Problems solved by technology

In previous reports (Shavel, A.; et.J.Phys.Chem.B 2004, 108, 5905-5908), the preparation of ZnS

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[0030] The microwave preparation method of water-soluble ZnSe quantum dots provided by the invention, the specific steps are as follows:

[0031] 1. Preparation of sodium selenium hydride NaHSe solution as selenium source: sodium borohydride NaBH with a molar ratio of 15:1 to 20:1 4 and selenium powder Se are placed in water, and left to react at room temperature for 24-60 hours to obtain NaHSe solution; Glutathione GSH solution, adjust the pH value of the solution to 8-12, inject NaHSe solution to obtain the ZnSe precursor solution, and store it under nitrogen protection; 3. Microwave the ZnSe precursor solution to obtain water-soluble ZnSe quantum dots, wherein the microwave heating conditions are: microwave power 50W-300W, heating time 1 minute-30 minutes, heating temperature 70-120 degrees Celsius, to obtain water-soluble ZnSe quantum dots with high fluorescence quantum efficiency.

[0032] Zinc salt or zinc oxide and hydroxide described in the present invention include: ...

Embodiment 1

[0049] Preparation of water-soluble ZnSe quantum dots I

[0050] (1) Preparation of NaHSe

[0051] 23.9 mg NaBH 4 Mix with 23.6 mg of Se powder, dissolve in 3 ml of ultrapure water, then keep the solution away from light, and store it at room temperature. 2 . After about 30 hours, the black Se powder disappeared and white Na appeared at the bottom of the bottle. 2 B 4 o 7 Precipitation, the supernatant is NaHSe solution, and the clear solution is separated for the preparation of ZnSe nanocrystals.

[0052] (2) Preparation of ZnSe precursor solution

[0053] 17.2 mg ZnCl 2 Dissolve in 100 ml of water, add 8.6 microliters of glutathione, adjust pH=11 with 0.5 mol / L NaOH solution, ZnCl 2 Mix the solution with GSH under vigorous stirring with N 2 The gas was deoxygenated for 30 minutes, and then 2 ml of NaHSe solution was injected as the ZnSe precursor solution.

[0054] (3) Preparation of ZnSe quantum dots by microwave irradiation

[0055] Take 20 ml of the ZnSe precur...

Embodiment 2

[0059] Preparation of water-soluble ZnSe quantum dots II

[0060] (1) Preparation of NaHSe

[0061] 17.5 mg NaBH 4 Mix with 20.1 mg of Se powder, dissolve in 3 ml of ultrapure water, then keep the solution away from light, and store it at room temperature. 2 . After about 48 hours, the black Se powder disappeared and white Na appeared at the bottom of the bottle 2 B 4 o 7 Precipitation, the supernatant is NaHSe solution, and the clear solution is separated for the preparation of ZnSe nanocrystals.

[0062] (2) Preparation of ZnSe precursor solution

[0063] 35.5 mg ZnCl 2 Dissolve in 100 ml of water, add 18.7 microliters of glutathione, adjust pH=8 with 0.5 mol / L NaOH solution, ZnCl 2 Mix the solution with GSH under vigorous stirring with N 2 The gas was deoxygenated for 30 minutes, and then 3 ml of NaHSe solution was injected as the ZnSe precursor solution.

[0064] (3) Preparation of ZnSe quantum dots by microwave irradiation

[0065] Take 20 ml of the ZnSe precur...

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Abstract

The invention discloses a microwave preparation method of water soluble ZnSe quantum dots, which comprises the following steps: (1) mixing solution of sodium hydrogen selenide with solution serving as a zinc source to obtain solution of ZnSe precursor; and (2) heating the solution of the ZnSe precursor by microwaves to obtain water soluble ZnSe quantum dots, wherein the microwave heating conditions include a microwave power of 50 to 300W, a heating time period of 1 to 30 minutes and a heating temperature of 70 to 120 DEG C and the solution serving as the zinc source may be solution of a zinc salt, zinc oxide or zinc hydroxide. The obtained high fluorescent quantum product has high yield, stability and water solubility and can be widely used for making fluorescent labels for biological detection and analysis.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials and biological analysis and detection, and in particular relates to a microwave preparation method of water-soluble ZnSe quantum dots. Background technique [0002] Quantum dots are a type of semiconductor nanocrystal grains composed of II-VI or III-V elements whose radius is smaller than or close to the exciton Bohr radius. Semiconductor nanocrystals have a quantum size effect, and their optical properties change with particle size. At the same time, their luminous efficiency is also greatly improved compared with bulk materials. In 1998, Alivisatos and Nie firstly reported the use of semiconductor nanocrystals instead of organic fluorescent dyes as biomolecular markers, and successfully labeled transferrin and immunoglobulin (Alivisatos, A.P.; et, Science 1998, 281, 2013- 2016; Nie, S.M.; et, Science 1998, 281, 2016-2018), heralding the great application potential of nanocrystals in...

Claims

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Application Information

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IPC IPC(8): C30B29/48C30B7/14C09K11/88
Inventor 汪联辉何耀赛丽曼陆昊婷
Owner 苏州市长三角系统生物交叉科学研究院有限公司
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