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Preparation method of quantum dot solution with core-shell structure

A quantum dot solution, core-shell structure technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of inability to directly use the biological field, difficult to obtain size quantum dots, low quantum yield, etc., to achieve a wide range of sizes, Reproducible and easy-to-use results

Inactive Publication Date: 2014-11-12
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Quantum dots synthesized by organic methods have a high quantum yield, but most of the reagents used are toxic and the synthesized quantum dots are hydrophobic, which cannot be directly used in the biological field. Therefore, more and more researches are turning to the aqueous phase method.
At present, the quantum dot solution made by the aqueous phase method has low quantum yield and poor stability, and it is difficult to obtain larger quantum dots.

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  • Preparation method of quantum dot solution with core-shell structure
  • Preparation method of quantum dot solution with core-shell structure
  • Preparation method of quantum dot solution with core-shell structure

Examples

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Embodiment 1

[0022] A preparation method of a core-shell structure quantum dot solution, the steps are as follows:

[0023] (1) Synthesis of CdTe quantum dot solution by aqueous phase method

[0024] Referring to the published literature Yang YH (Advanced Material, 2005, 17) or Gaponik, N (Journal of Physical Chemistry B, 2002, 106), the specific steps are:

[0025] Take 36.4mg NaBH 4 and 26.7mg of Te powder, add 1.5ml of double distilled water, and seal the reaction until the tellurium powder disappears completely, and the solution is light purple, which is the prepared NaHTe solution. Take 160mL of 0.026mol / L CdCl 2 solution, add 140 μL thioglycerol, 27.5 μL thioglycolic acid (TGA), and adjust the pH value of the solution to 11.2 with 1mol / L NaOH solution, heat the solution for 30 min in an oxygen-free environment, and quickly add freshly prepared NaHTe solution, and reacted at 97° C. for 1 h to obtain a CdTe quantum dot solution.

[0026] (2) The first step is to add NaOH to synthes...

Embodiment 2

[0032] A preparation method of a core-shell structure quantum dot solution, the steps are as follows:

[0033] (1) Synthesis of CdTe quantum dot solution by aqueous phase method

[0034] This step is the same as in Example 1.

[0035] (2) The first step is to add NaOH lye to synthesize quantum dots with core-shell structure

[0036] Take 1 mL of the newly synthesized CdTe quantum dot solution, add 1 mL of 0.2 mol / L NaOH solution, and react in a water bath at 96 °C for 4.5 h. At this time, the fluorescence emission wavelength of the quantum dot is 570nm, the size is about 3.7nm, and the quantum yield is 60%. The calculation of the quantum yield refers to the Brouwer method in 2011, using Rhodamine B as a reference, and the highest measured quantum dot The yield is 2-3 times that of the original quantum dot solution.

[0037] (3) Adding NaOH lye in two steps to synthesize quantum dots with core-shell structure

[0038] Take 1mL of 0.8mol / L NaOH solution and add it to the qua...

Embodiment 3

[0040] Jiang Guohui (Materials and Structure, 2012, 19) prepared CdSe quantum dot solution and other methods. Press CdCl 2 The molar ratio of thioglycolic acid and the stabilizer is 1:2.5, and the pH is adjusted to 10. KBH 4Add Se to deionized water at a molar ratio of 4:1, nitrogen protection, magnetic stirring, and reflux at 50°C for 20 min to obtain a clear sodium selenium hydride (KHSe) solution. To the prepared CdCl 2 Nitrogen was passed through the solution for 5-10 minutes, and then the KHSe solution was quickly injected into CdCl 2 In the solution, reflux reaction at 90° C. to obtain a quantum dot solution. The other steps of the lye method synthesis are the same as in Example 1 twice.

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Abstract

The invention discloses a preparation method of a quantum dot solution with a core-shell structure. The preparation method comprises the following steps of: (1) synthesizing quantum dots to obtain a quantum dot solution with concentration of 0.001-0.003 mol\L; and (2) adding NaOH solutions to the quantum dot solution for twice to react, wherein the concentration of the firstly added NaOH solution is 0.1-0.6 mol / L, the concentration of the secondly added NaOH solution is 0.8-1.2 mol / L, the volume ratio of the NaOH solution added for two reaction to the quantum dot solution is 1:1, the reaction is performed at 92-96 DEG C, and the time for each of two reaction is 1-6 hours. Compared with the prior art, the quantum dot with the core-shell structure prepared by the method disclosed by the invention is high in yield and good in stability and has a wide size range, and the surface hydrophilicity of the quantum dot can be directly applied to the biological field. The method further has the characteristics of simplicity in operation, low cost, good reproducibility, and the like.

Description

technical field [0001] The invention belongs to the technical field of semiconductor nanomaterials, and in particular relates to a preparation method of a quantum dot solution with a core-shell structure. technical background [0002] Quantum dots, also known as semiconductor nanocrystals, are mainly composed of chemical elements such as II-VI group (CdS, CdSe, CdTe, etc.) or III-V group elements (such as InP, InAs, etc.). Due to their small particle size (1-20nm), quantum dots have unique and superior optical, electronic and surface modification properties, and have become an upstart in the field of nano-biophotonics and are widely used in the field of biomarkers. [0003] A high-quality quantum dot solution has the following characteristics: a wide size range, a narrow size distribution, good stability, and high fluorescence. At present, the methods for synthesizing high-quality quantum dot solutions are mainly organic methods and aqueous phase methods. Quantum dots synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/88
Inventor 蔡朝霞王蓓蓓马美湖
Owner HUAZHONG AGRI UNIV