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Method for microwave-assisted preparation of CdTeSeS/ZnTe core-shell quantum dot in water

A core-shell quantum dot and microwave technology, which is applied in the field of nanomaterial technology, can solve the problems of inability to apply biomarkers, low quantum yield, and toxic ligands, and achieve easy control of process parameters, high quantum yield, and heating speed fast effect

Inactive Publication Date: 2015-10-14
天门市天宝化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the high-quality CdTeSeS quantum dots are all synthesized from the organic phase. The quantum dots directly synthesized in the aqueous phase not only have a wide half-peak width, but also have a relatively low quantum yield.
However, the ligands in the organic phase are toxic and cannot be applied to biomarkers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A CdTeSeS / ZnTe core-shell quantum dot, which consists of: selenium powder (Se, Tianjin Kemiou Chemical Reagent Development Center), sodium tellurite (NaTeO 3 , produced by Aladdin Chemical Reagent Co., Ltd., with a mass fraction of 97%), potassium borohydride (KBH 4 , Sinopharm Group Shanghai Chemical Reagent Co., Ltd., the mass fraction is 96%), cadmium chloride (CdCl 2 2.5H 2 O, Sinopharm Chemical Reagent Co., Ltd.), mercaptopropionic acid (MPA, Japan), and the rest were aqueous solutions.

[0025] In the described CdTeSeS / ZnTe core-shell quantum dots, sodium tellurite+sodium selenosulfate, cadmium chloride (CdCl 2 2.5H 2 O), the molar ratio of mercaptopropionic acid (MPA) is 1:2:4.8, the molar ratio of sodium tellurite to sodium selenosulfate is 1:1, heated at 130°C for 30min, the tellurous acid in the ZnTe shell material The molar ratio of sodium, cadmium chloride and mercaptopropionic acid (MPA) is 1:2:4.8, heated at 100°C for 40min, and the pH value is 8.

[...

Embodiment 2

[0037] A CdTeSeS / ZnTe core-shell quantum dot, which consists of: selenium powder (Se, Tianjin Kemiou Chemical Reagent Development Center), sodium tellurite (NaTeO 3 , produced by Aladdin Chemical Reagent Co., Ltd., with a mass fraction of 97%), potassium borohydride (KBH 4 , Sinopharm Group Shanghai Chemical Reagent Co., Ltd., the mass fraction is 96%), cadmium chloride (CdCl 2 2.5H 2 O, Sinopharm Chemical Reagent Co., Ltd.), mercaptopropionic acid (MPA, Japan), and the rest were aqueous solutions.

[0038] In the described CdTeSeS / ZnTe core-shell quantum dots, sodium tellurite+sodium selenosulfate, cadmium chloride (CdCl 2 2.5H 2 O), the molar ratio of mercaptopropionic acid (MPA) is 1:2:4.8, the molar ratio of sodium tellurite to sodium selenosulfate is 6:4, heated at 130°C for 40min, the tellurous acid in the ZnTe shell material The molar ratio of sodium, cadmium chloride and mercaptopropionic acid (MPA) is 1:2:4.8, heated at 100°C for 60min, and the pH value is 8.

[...

Embodiment 3

[0048] A water-phase microwave preparation method of CdTeSeS / ZnTe core-shell quantum dots, the steps are as follows:

[0049] 1. Weigh 2.3670g of selenium powder and 7.5624g of sodium sulfite in a 250mL three-neck flask, add 80mL of deionized water to it, and reflux in a water bath at 90°C for 8 or 9 or 10 hours until the solution is clear and transparent, and the black selenium powder disappears completely. The heat source stops heating. After naturally cooling to room temperature (20-25°C), transfer it to a 100mL volumetric flask and dilute it to the mark with deionized water, which is a 0.30mol / L sodium selenosulfate solution. The reaction equation is as follows:

[0050] Se+Na 2 SO 3 = Na 2 SeSO 3 ;

[0051] 2. Take 200 mL of oxygen-free deionized water, add 2.5 mL of 0.1 mol / L cadmium chloride solution and 5.76 mL of 0.1 mol / L mercaptopropionic acid solution in turn, and adjust the pH value with 1 mol / L sodium hydroxide solution 8. Add 22.4g of sodium tellurit...

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Abstract

The invention relates to a method for microwave-assisted preparation of a CdTeSeS / ZnTe core-shell quantum dot in water. The method comprises the following steps: 1) preparing a sodium elenosulfate solution; 2) preparing a cadmium chloride solution; 3) adding mercaptopropionic acid into the cadmium chloride solution; 4) adjusting the pH value of the solution; 5) dissolving a sodium tellurite crystal in the solution and simultaneously adding potassium borohydride and the sodium elenosulfate solution; 6) subjecting a mixture obtained in the step 6) to heating reaction in a microwave digestion furnace; 7) carrying out cooling to room temperature and adding isopropanol for purification so as to obtain CdTeSeS quantum dot gel; and 8) preparing a mixed solution of the cadmium chloride solution, the mercaptopropionic acid and the sodium tellurite crystal, dissolving the CdTeSeS quantum dot gel in the mixed solution anew, adding potassium borohydride and successively carrying out heating reaction in the microwave digestion furnace, cooling to room temperature, addition of isopropanol for purification and drying with a lyophilizer so as to obtain solid powder of the CdTeSeS / ZnTe core-shell quantum dot. The method is fast and simple and has easily controllable technological parameters and a low price; and the synthesized quantum dot has uniform particle size distribution, high stability, high fluorescence quantum yield and wide emission spectrum.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and relates to the synthesis of fluorescent nanomaterials, in particular to a water-phase microwave preparation method of CdTeSeS / ZnTe core-shell quantum dots. The quantum efficiency is high, and it can be directly used for cell imaging and living body labeling, and can also be used for the detection of heavy metal ions such as Hg and Cu in water. Background technique [0002] CdTeSeS quaternary alloy quantum dots have the characteristics of adjustable luminescence characteristics, the luminescence range covers from green light to near-infrared light region, wide excitation range, relatively narrow emission full width at half maximum, and high luminescence quantum yield. It has become one of the quantum dots with the most research value. The most rare thing is that by adjusting the ratio of Te and Se, the excitation wavelength of quantum dots can be adjusted at will, reaching the near-in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/88
Inventor 刘西京
Owner 天门市天宝化工科技有限公司
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