Preparation method of pure yellow fluorescence water-soluble doped zinc selenide quantum dots

A yellow fluorescent, water-soluble technology, applied in chemical instruments and methods, luminescent materials, etc., to achieve good water solubility, simple operation, and low cost

Inactive Publication Date: 2015-02-04
SOUTHEAST UNIV
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Problems solved by technology

[0004] The purpose of the invention is to provide a method for preparing pure yellow fluorescent water-soluble doped zinc selenide quantum dots, to solve the existing problem of using water as a solvent to prepare internally doped water-soluble Mn:ZnSe quantum dots with multiple fluorescence peaks

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[0020] A preparation method of pure yellow fluorescent water-soluble doped zinc selenide quantum dots, comprising the steps of:

[0021] Step 1. Add 0.1mol / LMnCl to deionized water 2 Solution, 0.1mol / LAgNO 3 The solution and the ligand (mercaptoacetic acid or mercaptopropionic acid) containing mercapto groups are mixed evenly, and the pH is adjusted to 7.1 to 12.5, preferably 11.9, with 5mol / L sodium hydroxide solution to obtain an aqueous solution of impurity ion precursor; wherein, Mn 2+ and Ag + The molar ratio of Mn is 1:0.5~2, preferably 1:1.5, Mn 2+ The molar ratio to the ligand containing thiol is 1:20-50, preferably 1:37.3, Mn 2+ The concentration is 4×10 -5 mol / L. The solution cannot be left for a long time and should be used immediately after preparation.

[0022] Step 2. Under the ice bath, deoxygenate the impurity ion precursor aqueous solution prepared in step 1 with nitrogen gas, and the deoxygenation time is not less than 10 minutes. After that, NaHSe aque...

Embodiment 1

[0029] 1. Add 0.1mol / L MnCl to 200mL deionized water 2 Solution 80uL, 0.1mol / L AgNO 3 120 uL of the solution, followed by 26 uL of mercaptopropionic acid, stirred for 1 minute and then adjusted the pH of the mixed solution to 11.9 with 5 mol / L NaOH solution to obtain an aqueous solution of impurity ion precursor. This solution cannot be left for a long time, and it should be used immediately after preparation.

[0030] 2. Add the above-mentioned newly prepared impurity ion precursor solution into a round bottom flask with a capacity of 250mL, place the round bottom flask in an ice-water bath to cool for 30min, and deoxygenate the solution with high-purity nitrogen at the same time. After the temperature of the solution was cooled to 0°C, 0.25 mL of NaHSe aqueous solution with a concentration of 0.667 mol / L was quickly extracted with a syringe and injected into the above-mentioned flask under rapid stirring, and stirred for 5 min.

[0031] 3. Transfer the above-mentioned roun...

Embodiment 2

[0036] 1. Add 0.1mol / L MnCl to 200mL deionized water 2 Solution 80uL, 0.1mol / L AgNO 3 40 uL of the solution, followed by injection of 14 uL of mercaptopropionic acid, and after stirring for 1 minute, the pH of the mixed solution was adjusted to 7.1 with 5 mol / L NaOH solution to obtain an aqueous solution of impurity ion precursor. This solution cannot be left for a long time, and it should be used immediately after preparation.

[0037] 2. Add the above-mentioned newly prepared impurity ion precursor solution into a round bottom flask with a capacity of 250mL, place the round bottom flask in an ice-water bath to cool for 30min, and deoxygenate the solution with high-purity nitrogen at the same time. After the temperature of the solution was cooled to 0°C, 0.073 mL of NaHSe aqueous solution with a concentration of 0.667 mol / L was quickly extracted with a syringe and injected into the above flask under rapid stirring, and stirred for 5 min.

[0038] 3. Transfer the above-menti...

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Abstract

The present invention discloses a preparation method of pure yellow fluorescence water-soluble doped zinc selenide quantum dots, wherein Mn:ZnSe quantum dots are doped with another impurity Ag<+>, such that the intrinsic fluorescence and the defect fluorescence of the ZnSe quantum dots are inhibited while the original intensity of the impurity fluorescence of Mn is maintained so as to prepare the pure Mn yellow fluorescence doped ZnSe quantum dots, and the prepared quantum dots have good water solubility and good fluorescence stability, and only have the one strong Mn fluorescence emission peak. According to the present invention, the one-step synthesis of the pure yellow fluorescence doped ZnSe quantum dots in the aqueous solution is achieved, and the preparation method has advantages of simple operation, good repeatability, green environmental protection, low cost and the like, and can be used for mass production of the quantum dots.

Description

technical field [0001] The invention relates to the field of preparation of water-soluble quantum dots, in particular to a preparation method of pure yellow fluorescent water-soluble doped zinc selenide quantum dots. Background technique [0002] Water-soluble Mn:ZnSe quantum dots have the advantages of non-toxicity and strong biocompatibility. When using the traditional doping method to prepare Mn:ZnSe quantum dots, Mn impurities are often located on the surface of the quantum dots. This type of surface-doped quantum dots has poor stability, and its fluorescence is easy to change with the surrounding environment. The nucleation doping method developed in 2005 has better solved the above shortcomings. In this method, the Mn impurity is directly used as a nucleus to grow ZnSe, thereby confining Mn inside the quantum dot. Such internally doped quantum dots have good fluorescence stability. [0003] So far, there are two main methods for preparing internally doped water-sol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/58
Inventor 王春雷胡志扬徐淑宏崔一平
Owner SOUTHEAST UNIV
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