Preparation method of Cu-Mn double-doping ZnS quantum dot solution and application

A quantum dot solution and double-doping technology, which is applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve the problem of instability of the dual emission wavelength system of fluorescent probes, and achieve stable optical properties and fluorescent optical properties. Adjustable, good water solubility

Active Publication Date: 2017-08-04
NORTHWEST UNIV(CN)
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Problems solved by technology

[0004] Aiming at the defects and deficiencies of the existing preparation technology, the present invention provides a method for phase preparation of Cu-Mn double-doped ZnS quantum dot ratio fluorescent probe, which solves the problem of instability of the existing fluorescent probe dual emission wavelength system, A Cu-Mn dual-doped ZnS quantum dot ratiometric fluorescent probe synthesized in aqueous phase with good water solubility and tunable fluorescence

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  • Preparation method of Cu-Mn double-doping ZnS quantum dot solution and application
  • Preparation method of Cu-Mn double-doping ZnS quantum dot solution and application
  • Preparation method of Cu-Mn double-doping ZnS quantum dot solution and application

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[0028] The preparation method of Cu-Mn double-doped ZnS quantum dot solution of the present invention comprises the following steps:

[0029] Step 1: Add Zn 2+ solution and containing Mn 2+ The solution is mixed, then the organic ligand is added and stirred evenly, and the pH value is adjusted to 10-11 with NaOH solution to obtain a mixed solution;

[0030] Step 2: Add S to the mixture obtained in Step 1 2- solution, reacting at 80-100°C for 1-2 hours to obtain a Mn-doped ZnS nanocrystal solution;

[0031] Step 3: Add Cu containing Cu to the Mn-doped ZnS nanocrystal solution obtained in Step 2 2+ The solution is reacted at 80-100° C. for 20-30 minutes, and air-cooled to room temperature to obtain a Cu-Mn double-doped ZnS quantum dot solution. Contains Cu 2+ The addition rate of the solution is generally controlled at 0.3-0.6mL / min to ensure that the Cu 2+ The ions are uniformly doped in the quantum dot crystal.

[0032] Among them: containing Zn 2+ The solution of Zn(C...

Embodiment 1

[0051] 1mmol of Zn(CH 3 COO) 2 , 2mmol of glutathione and a certain amount of 0.1mol / LMn(CH 3 COO) 2 The solution was added into a three-necked flask, and 100 mL of deionized water was added and stirred until the system was clear. Then use 1mol / L NaOH solution to adjust the pH value of the system to 10, raise the temperature to 60°C and continue stirring for 20min, then add 10mL freshly prepared 0.1mol / L NaOH dropwise. 2 S solution. After adding Na 2 After the S solution, the temperature of the system was raised to 100°C and kept at this temperature for 2 hours. At this time, a certain amount of 0.1mol / L Cu(CH 3 COO) 2 The solution was slowly added to the reaction system, the drip rate was controlled at 0.3-0.6mL / min through the infusion set, and the ratio range of the doping ion Cu / Mn was 1:0.1. After continuing the reaction for 30 min, the heating device was removed, and the reaction system was naturally cooled to room temperature to obtain a Cu-Mn double-doped ZnS qu...

Embodiment 2

[0053] 1mmol of Zn(CH 3 COO) 2 , 2mmol of cysteine ​​and a certain amount of 0.1mol / LMn(CH 3 COO) 2 The solution was added into a three-necked flask, and 100 mL of deionized water was added and stirred until the system was clear. Then adjust the pH value of the system to 11 with 1mol / L NaOH solution, raise the temperature to 60°C and continue to stir for 20min, then add 10mL of freshly prepared 0.1mol / L NaOH dropwise. 2 S solution. After adding Na 2 After the S solution, the temperature of the system was raised to 80°C and kept at this temperature for 2h. At this time, a certain amount of 0.1mol / L Cu(CH 3 COO) 2 The solution was slowly added to the reaction system, the drip rate was controlled at 0.3-0.6mL / min through an infusion set, and the ratio of doping ions Cu / Mn was in the range of 1:1.0. After continuing to react for 20 min, the heating device was removed, and the reaction system was naturally cooled to room temperature to obtain a Cu-Mn double-doped ZnS quantum...

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Abstract

The invention discloses a preparation method of a Cu-Mn double-doping ZnS quantum dot solution and application. Firstly, Mn-doped ZnS nanometer crystals are obtained in the nucleation doping process, i.e., Mn precursors and Zn precursors are mixed and are added into S precursors; after the reaction for a period of time, Cu precursors are added; the reaction temperature is controlled, so that the crystals continuously grow; therefore Cu-Mn double-doping ZnS quantum dots are obtained. The prepared double-doping quantum dots simultaneously have Cu and Mn doping fluorescence emission peaks; in addition, the Cu doping fluorescence emission peak is sensitive to the environment and can be used as recognition signals; the Mn doping fluorescence emission peak is used as a reference signal. Therefore the obtained Cu-Mn double-doping ZnS quantum dots can be used as ratio fluorescent probes for analysis and detection. The preparation method disclosed by the invention has the advantages that the preparation method is simple; a green effect is achieved; the repeatability is good; the prepared double-doping ZnS quantum dots have good water solubility; the fluorescence is adjustable.

Description

technical field [0001] The invention belongs to the technical field of fluorescent probe preparation, and in particular relates to a preparation method and application of a Cu-Mn double-doped ZnS quantum solution. Background technique [0002] Fluorescent signals are widely used in the field of analysis and detection due to their high sensitivity and easy detection. Traditional fluorescent probes are mainly organic fluorescent dyes, which use the response of chromophores to target detection substances to achieve quantitative detection. In recent years, with the development of nanotechnology, nanofluorescent materials have been applied in the field of analysis and detection due to their excellent properties such as high fluorescence quantum yield, stable chemical properties, anti-photobleaching, and adjustable fluorescence. Fluorescent probes based on semiconductor quantum dots (Quantum dots, QDs), noble metal nanoclusters (Au, Ag Nanoclusters), carbon dots (Carbon dots, CDs)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/56G01N21/64
Inventor 樊君王永波刘恩周贾丽从聂齐齐胡晓云
Owner NORTHWEST UNIV(CN)
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