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Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot

A water-phase preparation, water-soluble technology, applied in chemical instruments and methods, nanotechnology, nano-optics and other directions, can solve the problems of cumbersome preparation steps, large amount of cadmium, scarcity, etc., and achieves cheap and easy to obtain raw materials, short reaction time, The effect of high reaction temperature

Inactive Publication Date: 2015-06-17
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the lack of synthesis of chiral ZnCdSe quantum dots at present, and the large amount of cadmium used in the preparation of water-soluble ZnCdSe quantum dots, the preparation steps are cumbersome and other problems, the present invention provides a safe and convenient way to synthesize high-quality water-soluble chiral ZnCdSe quantum dots The aqueous phase preparation method

Method used

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  • Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot
  • Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot
  • Aqueous phase preparation method for water-soluble chiral ZnCdSe quantum dot

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 1. Prepare KHSe solution: mix 20mg selenium powder and 40mgKBH 4 Mixed, inject 3mL deionized water, stir and react at 25°C for 45min to obtain KHSe solution.

[0054] 2. Prepare the precursor solution of zinc in the two-necked flask, with 24.5mgZnCl 2 and 88.0mg N-acetyl-L-cysteine ​​were dissolved in 50mL deionized water, and the pH value of the solution was adjusted to 8~11 with 1mol / L NaOH to prepare a zinc precursor solution, wherein [Zn 2+ ]=3.6mmol / L; The molar ratio of Zn and N-acetyl-L-cysteine ​​is 1:3.

[0055] 3. Pass argon for 20 minutes to remove the oxygen in the zinc precursor solution, quickly inject 213 μL of the KHSe solution prepared in step 1, and 1 mL of 3.6 mmol / L CdCl 2 solution. After mixing, transfer to a hydrothermal reaction kettle, heat to 200° C. in an oven, and react for 60 minutes to obtain a solution of ZnCdSe quantum dots coated with water-soluble chiral N-acetyl-L-cysteine.

[0056] 4. Add 2 times the volume of ethanol to the obtain...

Embodiment 2

[0058] 1. Prepare KHSe solution: mix 10mg selenium powder and 25mgKBH 4 Mix, inject 3mL of deionized water, and stir the reaction at 20°C for 46min to obtain a KHSe solution.

[0059] 2. Prepare the precursor solution of zinc in the two-necked flask, with 24.5mgZnCl 2 and 88.0mg N-acetyl-L-cysteine ​​were dissolved in 50mL deionized water, and the pH value of the solution was adjusted to 9.7 with 1mol / L NaOH to prepare a zinc precursor solution, wherein [Zn 2+ ]=3.6mmol / L; The molar ratio of Zn and N-acetyl-L-cysteine ​​is 1:3.

[0060] 3. Nitrogen was passed for 35 minutes to remove the oxygen in the zinc precursor solution, and 426 μL of the KHSe solution prepared in step 1 and 1 mL of 3.6 mmol / L CdCl were quickly injected 2 solution. After mixing, transfer to a hydrothermal reaction kettle, heat to 200° C. in an oven, and react for 50 to 70 minutes to obtain a water-soluble chiral N-acetyl-L-cysteine-wrapped ZnCdSe quantum dot solution.

[0061] 4. Add 2 times the volum...

Embodiment 3

[0063] 1. Prepare NaHSe solution: mix 10mg selenium powder and 11mgNaBH 4 After mixing, inject 3 mL of deionized water, and stir the reaction at 15°C for 100 min to obtain a NaHSe solution.

[0064] 2. Prepare the precursor solution of zinc in the two-necked flask, with 24.5mgZnCl 2 35.2 mg, 58.7 mg, 70.4 mg, 88.0 mg and 105.6 mg of N-acetyl-L-cysteine ​​were mixed and dissolved in 50 mL of deionized water, and the pH value of the solution was adjusted to 9.7 with 1 mol / L NaOH to prepare Get the precursor solution of zinc, wherein [Zn 2+]=3.6mmol / L; the molar ratios of Zn and N-acetyl-L-cysteine ​​were 1:1.2, 1:2.0, 1:2.4, 1:3.0, 1:3.6, respectively.

[0065] 3. Nitrogen gas was passed for 40 minutes to remove the oxygen in the zinc precursor solution, and 426 μL of the NaHSe solution prepared in step 1 and 1 mL of 3.6 mmol / L CdCl were quickly injected 2 solution. After mixing, transfer to a hydrothermal reaction kettle, heat to 200° C. in an oven, and react for 60 minutes...

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Abstract

The invention discloses an aqueous phase preparation method for a water-soluble chiral ZnCdSe quantum dot. The preparation method comprises the following steps: (a) preparing a NaHSe or KHSe solution as a selenium source solution, dissolving a zinc salt and a water-soluble chiral mercapto compound in water so as to obtain a precursor solution of zinc and preparing an aqueous solution of a cadmium salt; (b) blowing inert gas into the precursor solution of zinc, injecting the selenium source solution and the aqueous solution of the cadmium salt and carrying out stirring so as to prepare a ZnCdSe precursor solution; and (c) subjecting the ZnCdSe precursor solution to a reflux reaction under stirring at a temperature of 80 to 100 DEG C for 1 to 5 h under the protection of inert gas, or transferring the ZnCdSe precursor solution to a reaction vessel and heating the ZnCdSe precursor solution to 160 to 210 DEG C for a reaction for 45 to 90 min so as to prepare an aqueous solution of the water-soluble chiral ZnCdSe quantum dot. The preparation method substantially reduces the usage amount of cadmium and is safe, simple and convenient to operate; and the obtained quantum dot has excellent photochemical properties and chirality and has wide application prospects in aspects like detection, location and targeted tracing of chiral substances.

Description

technical field [0001] The invention relates to the fields of nanomaterial preparation technology and biological analysis and detection technology, in particular to a water-phase preparation method of water-soluble chiral ZnCdSe quantum dots. Background technique [0002] Quantum dots (quantum dots, QDs) are quasi-zero-dimensional nanomaterials composed of II-VI or III-V elements, with a diameter between 1 and 10 nm, and composed of a relatively small number of atoms or molecules. . It has an atomic-like physical structure, and also has a molecular-like quasi-discrete energy level. Because its diameter is close to the wavelength of light, quantum dots can produce special interactions with light. The ultraviolet-visible broad spectrum of quantum dots has many energy levels, and many electronic states exist at higher energy levels, thus allowing a single wavelength of light to simultaneously excite multi-color quantum dots. Varying the size and composition of quantum dots ca...

Claims

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Application Information

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IPC IPC(8): C09K11/88C09K11/02B82Y40/00B82Y20/00
Inventor 赵丹郝健
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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