Preparation method of water soluble manganese added zinc sulfide nano-crystalline with high fluorescence efficiency

A nanocrystalline, water-soluble technology, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problem of high fluorescence quantum yield of products, achieve high fluorescence efficiency, good water solubility, and simple operation

Inactive Publication Date: 2006-01-18
JILIN UNIV
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Problems solved by technology

[0009] The technical problem to be solved in the present invention is, aiming at the defects of the present ZnS:Mn nanocrystal aqueous phase co-precipitation synthesis method, establish a kind of high fluorescence efficiency water-soluble ZnS:Mn nanocrystal microwave-assisted synthesis method, make this method have the operation Simple, mild synthesis conditions, fast reaction speed, good repeatability, etc., the obtained product has high fluorescence quantum yield and good water solubility

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Synthesis of ZnS:Mn nanocrystal precursor:

[0019] Utilize mercaptopropionic acid as a stabilizer, use water as a solvent, mix the 0.1 mol / liter manganese salt solution and the zinc salt solution according to the molar ratio of 3:100, and then add mercaptopropionic acid with a molar ratio of 1:4 to the zinc salt acid, adjust the pH of the solution to 10.3, and then inject the sodium sulfide solution, Zn 2+ / S 2- The molar ratio is 1:0.9. React at room temperature for 15 minutes. The obtained ZnS:Mn nanocrystal precursor has a hydrosol fluorescence quantum yield of 2.1%.

[0020] (2) Zinc mercapto complex preparation:

[0021] Mix 5 milliliters of 0.1 mol / liter of zinc acetate aqueous solution and 15 milliliters of 0.1 mol / liter of mercaptopropionic acid aqueous solution, the mol ratio of zinc salt and mercaptopropionic acid is 1: 3, the pH value of mixed solution is adjusted to Turn it up to 9.

[0022] (3) Microwave hydrothermal synthesis of ZnS:Mn nanocryst...

Embodiment 2

[0028] (1) Synthesis of ZnS:Mn nanocrystal precursor: synthesized according to the method described in Example 1.

[0029] (2) Mix 5 milliliters of 0.1 mol / liter zinc acetate aqueous solution with 25 milliliters of 0.1 mol / liter mercaptopropionic acid (MPA) aqueous solution, the molar ratio of zinc salt and mercaptopropionic acid is 1:5, and use sodium hydroxide solution Adjust the pH of the mixture to 10.8.

[0030] (3) Microwave hydrothermal synthesis of ZnS:Mn nanocrystals with high fluorescence efficiency:

[0031] The ZnS obtained in step (1): the Mn nanocrystal precursor sol is made into the aqueous solution that Zn concentration is 0.01 mol / liter, and the mercapto complex compound of zinc in step (2) is made into Zn concentration with water and is 0.01 mol / liter of aqueous solution. Get 30 milliliters of 0.01 mol / liter ZnS: the aqueous solution of Mn nanocrystal is diluted to 130 milliliters, then add 20 milliliters of concentrations and be the mercapto complex soluti...

Embodiment 3

[0036] The zinc acetate aqueous solution among the embodiment 1 or 2 is replaced with the aqueous solution of zinc nitrate or zinc chloride, all the other reaction processes and conditions are constant, and the obtained result is identical with embodiment 1 or 2.

[0037] The aqueous solution of mercaptopropionic acid in embodiment 1 or 2 is replaced with aqueous solution of mercaptoacetic acid, and all the other reaction processes and conditions are constant, and obtained result is identical with embodiment 1 or 2.

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Abstract

The present invention is the preparation process of nanometer ZnS:Mn crystal with high fluorescent efficiency and high water solubility and belongs to the field of nanometer material preparing technology. After the water soluble nanometer ZnS:Mn crystal precursor synthesized through co-precipitation process and one kind of zinc mercapto complex are set inside microwave reactor, the zinc mercapto complex is decomposed under microwave heating condition and one layer of zinc sulfide is grown on the surface of the ZnS:Mn crystal precursor, so as to improve the dispersion state of Mn ions inside nanometer ZnS crystal and obtain nanometer ZnS:Mn crystal with high fluorescent efficiency. The process has simple operation and mild reaction condition, and the synthesized nanometer ZnS:Mn crystal has excellent water solubility and relatively high fluorescent quantum efficiency.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing water-soluble manganese-doped zinc sulfide nanocrystals by using microwave-assisted synthesis technology. Background technique [0002] In the past ten years, the application of fluorescent nanocrystals in biomarkers has attracted more and more attention. Compared with traditional organic dyes, fluorescent nanocrystals have better optical properties. Its excitation wavelength is wider and its emission wavelength is narrower, which is convenient for multi-index joint detection of fluorescence; it has high quantum yield and strong anti-light Oxidation and photobleaching ability. Connecting nanocrystals with biomacromolecules to form bioluminescent probes has broad application prospects in biotechnology fields such as immunoassays, fluorescence imaging of living tissues, clinical diagnosis, and drug screening. [0003] In 1994, N...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/48C30B7/14
Inventor 杨文胜菅文萍庄家骐王刚白玉白
Owner JILIN UNIV
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