Method for water-phase microwave preparation of CdSeS quantum dots

A quantum dot and microwave technology, which is applied in the field of synthesis of fluorescent nanomaterials, can solve the problems of inability to apply biomarkers, low quantum yield, and half-peak width, etc., and achieve easy control of process parameters, simplified synthesis steps, and small particle size Effect

Inactive Publication Date: 2012-06-27
WUHAN UNIV
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Problems solved by technology

However, the high-quality CdSe quantum dots currently synthesized are all synthesized from the organic phase. The quantum dots directly s...

Method used

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Embodiment 1

[0023] Below by embodiment, further illustrate outstanding feature of the present invention, only in order to illustrate the present invention and in no way limit the present invention.

[0024] A kind of CdSeS alloy quantum dot, it is composed of: selenium powder (Se, Tianjin Kemiou Chemical Reagent Development Center), cadmium chloride (CdCl 2 2.5H 2 0, Sinopharm Chemical Reagent Co., Ltd.), mercaptopropionic acid (MPA, Japan), and the rest were aqueous solutions.

[0025] In the described CdSeS alloy quantum dots, selenium powder (Se), cadmium chloride (CdCl 2 2.5H 2 O), the molar ratio of mercaptopropionic acid (MPA) is 0.2: 1: 2.0, and heated at 120-150° C. for 20-40 min.

[0026] The pH of the solution is 8-10.

[0027] A microwave-assisted synthesis method of CdSeS alloy quantum dots, the steps are:

[0028] 1. Selenium powder (Se) and sodium sulfite (Na 2 SO 3 ) reaction to prepare sodium selenosulfate solution: Weigh 2.3670g of selenium powder and 7.5624g of so...

Embodiment 2

[0035] A kind of CdSeS alloy quantum dot, it is composed of: selenium powder (Se, Tianjin Kemiou Chemical Reagent Development Center), cadmium chloride (CdCl 2 2.5H 2 O, Sinopharm Chemical Reagent Co., Ltd.), mercaptopropionic acid (MPA, Japan), and the rest were aqueous solutions.

[0036] In the described CdSeS alloy quantum dots, sodium selenosulfate (Na 2 SeSO 3), cadmium chloride (CdCl 2 2.5H 2 O), the molar ratio of mercaptopropionic acid (MPA) is 0.125: 1: 2.4, heated at 130° C. for 30-40 min.

[0037] The pH of the solution is 9-9.5.

[0038] A microwave-assisted synthesis method of CdSeS alloy quantum dots, the steps are:

[0039] 1. Weigh 1.1835g of selenium powder and 3.7812g of sodium sulfite into a 250mL three-neck flask, add 85mL of deionized water, and reflux in a water bath at 95°C for 8 or 9 or 10 hours until the solution is clear and transparent. Remove the heat source and stop heating. After naturally cooling to room temperature (20-25°C), transfer it...

Embodiment 3

[0045] 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:

[0046] Se+Na 2 SO 3 =Na 2 SeSO 3 ;

[0047] 2. Take 200 mL of anaerobic deionized water, add 2.5 mL of 0.10 mol / L cadmium chloride solution, 6 mL of 0.10 mol / L mercaptopropionic acid solution, and adjust the pH value to 8 with 5 mol / L sodium hydroxide solution. Or 9 or 10, add 0.166mL0.30mol / L sodium selenosulfate solution after 30min of nitrogen gas, and continue to ventilate for 5min;

[0048] 3. The above mixed liquid wa...

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Abstract

The invention discloses a method for water-phase microwave preparation of CdSeS quantum dots. The method provided by the invention comprises the following steps of 1, preparing a selenosulfate solution through the reaction of selenium powder and a sodium sulfite solution, 2, weighing cadmium chloride crystals, and carrying out dissolution and volume metering by deionized water to obtain a cadmium chloride solution, 3, adding a certain amount of mercaptopropionic acid into the cadmium chloride solution, 4, adjusting a pH value of the mixed solution obtained by the step 3 to a specific pH value by a sodium hydroxide solution, 5, feeding inert gas into the mixed solution having the specific pH value to remove oxygen, and adding the selenosulfate solution obtained by the step 1 into the oxygen-free mixed solution, 6, loading the mixed solution obtained by the step 5 into a teflon-made digestion tank, and heating for a reaction by a microwave digestion furnace, and 7, cooling the reaction products obtained by the step 6 to a room temperature, adding isopropanol into the cooled reaction products, carrying out purification, and drying by a freezer dryer to obtain solid powder of the CdSeS quantum dots. The method provided by the invention is fast and simple, has easily controllable technological parameters, has a low cost, realizes small sizes and even size distribution of the CdSeS quantum dots obtained by the method, and has a high fluorescent quantum yield. The CdSeS quantum dots obtained by the method can be utilized as a biological fluorescent label material through coupling with biomolecules and can also be utilized for metal ion detection.

Description

technical field [0001] The present invention relates to the synthesis of fluorescent nanomaterials, more specifically to a water-phase microwave preparation method of CdSeS quantum dots, the synthesized quantum dots have a small particle size (2-4nm) and uniform particle size distribution, and the fluorescence quantum efficiency is relatively high. Finally, it can be used as a bioluminescent labeling material, and can also be used for the detection of metal ions. Background technique [0002] CdSe quantum dots have the characteristics of tunable luminescence characteristics (the luminescence range covers the entire visible region from blue to red light), wide excitation range, relatively narrow emission full width at half maximum, and high luminescence quantum yield. One of the most studied quantum dots. However, the high-quality CdSe quantum dots currently synthesized are all synthesized from the organic phase, and the quantum dots directly synthesized in the aqueous phase...

Claims

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Application Information

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IPC IPC(8): C09K11/88
Inventor 周培疆詹红菊丁玲何振宇
Owner WUHAN UNIV
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