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A kind of preparation method of cdse/cds/zns core-shell structure quantum dot

A technology of core-shell structure and quantum dots, which is applied in the field of preparation of CdSe/CdS/ZnS core-shell structure quantum dots, can solve the problems of quantum dot luminescence peak position control, high cost of quantum dots, difficulties, etc. Sensitive, easy to weigh, effect of reducing toxicity

Active Publication Date: 2019-03-29
周一飞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Under industrial production conditions, different batches of quantum dots are required to maintain consistency, which requires good repeatability in the synthesis of quantum dots. However, because quantum dot luminescence is extremely sensitive to size, this leads to control over the position of quantum dot luminescence peaks. This is one of the reasons why the cost of quantum dots remains high when applied on a large scale

Method used

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  • A kind of preparation method of cdse/cds/zns core-shell structure quantum dot
  • A kind of preparation method of cdse/cds/zns core-shell structure quantum dot
  • A kind of preparation method of cdse/cds/zns core-shell structure quantum dot

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preparation example Construction

[0037] A preparation method of CdSe / CdS / ZnS core-shell structure quantum dots, the steps are as follows:

[0038] S1, put the cadmium source and the selenium source into the ODE solution and mix, stir and heat; the concentration of Se is 0.075-0.15mol / L. The selenium source is SeO 2 , Se; the cadmium source is a mixture of cadmium stearate or cadmium oxide / salt and excess surfactant. The molar ratio of Se to Cd is: Se:Cd=1:1-5, preferably: Se:Cd=1:1.5-2.

[0039] S2, under stirring, heat to the preset temperature (190°C-200°C) and start timing. After reaching the predetermined time, slowly inject ODE-S solution, then inject OLA, and start growing quantum dots; the preparation process of the ODE-S solution For: dissolve sulfur powder in octadecene to make ODE-S solution. The estimated time is 20s-4min, preferably 1min.

[0040] The concentration of S in the ODE-S solution in this step is 0.1-0.5 mol / L.

[0041] The molar ratio of S in this step to Se in step S1 is: S:Se=1-...

Embodiment 1

[0050] (1) Preparation of stock solution: 4 mg of sulfur powder was dissolved in 1 mL of octadecene to obtain ODE-S solution;

[0051] (2) Mix 101.9 mg cadmium stearate and 7.9 mg selenium powder in 5 mL of ODE solution, stir and heat under nitrogen atmosphere;

[0052] (3) Under stirring, heat to 200°C and start timing, slowly inject ODE-S stock solution after 1 minute, and then inject OLA 0.0mL;

[0053] (4) After the reaction is carried out to the first 4 minutes, the temperature is rapidly cooled to room temperature, and the reaction is terminated;

[0054] (5) The reaction stock solution of step (4) obtains quantum dots through aftertreatment, and the quantum dots obtained are dissolved in toluene;

[0055] (6) Dissolve 9 mg of sulfur powder in 1 mL of octadecene to make ODE-S solution and transfer it into a syringe for later use;

[0056] (7) Mix 16.5mg of zinc acetate, 1mL of OA, and 5mL of ODE and heat it to above 280°C and keep it warm for a certain period of time t...

Embodiment 2

[0062] (1) Preparation of stock solution: 4 mg of sulfur powder was dissolved in 1 mL of octadecene to obtain ODE-S solution;

[0063] (2) Mix 84.9mg cadmium stearate with 11.1mg SeO 2 Mix in 5mL of ODE solution, stir and heat under nitrogen atmosphere;

[0064] (3) Under stirring, heat to 200°C and start timing, and slowly inject ODE-S stock solution after 4 minutes, and then inject OLA 0.3mL;

[0065] (4) Sampling is carried out in the 4th minute after the reaction is carried out, and the temperature is rapidly cooled to room temperature in the 6th minute after the reaction is carried out, and the reaction is terminated;

[0066] (5) The reaction stock solution of step (4) obtains quantum dots through aftertreatment, and the quantum dots obtained are dissolved in toluene;

[0067] (6) Dissolve 9 mg of sulfur powder in 1 mL of octadecene to make ODE-S solution and transfer it into a syringe for later use;

[0068] (7) Mix and heat 16.5mg of zinc acetate, 1mL OA, and 5mL OD...

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Abstract

The invention discloses a preparation method of a CdSe / CdS / ZnS core-shell structure quantum dot. The preparation method comprises steps as follows: S1, a cadmium source and a selenium source are put in an ODE solution to be mixed, and the mixture is stirred and heated; S2, when the mixture is heated to the preset temperature, timing starts, the ODE-S solution and OLA are injected sequentially after preset time is up, and growth of the quantum dot starts; S3, when the quantum dot grows to a predicted size, the quantum dot is cooled to the room temperature, and the quantum dot is obtained; S4, the quantum dot obtained in S3 is dissolved in toluene; S5, a zinc source, OA and ODE are mixed and heated to 280 DEG C or above, thermal insulation is performed, and cooling is performed after the solution becomes clear and transparent; S6, part of the quantum dot in S4 is injected into a reaction solution in S5, and the mixture is stirred and heated to be kept at the temperature for thermal insulation in S5; S7, the reaction solution in S4 is injected for set time, the ODE-S solution is injected, a reaction is performed at the temperature for thermal insulation in S5, and the CdSe / CdS / ZnS core-shell structure quantum dot is obtained. The CdSe / CdS / ZnS core-shell structure quantum dot has good repeatability and reliable product performance.

Description

technical field [0001] The invention relates to the technical field of semiconductors and luminescent nanometer materials, in particular to a preparation method of CdSe / CdS / ZnS core-shell structure quantum dots. Background technique [0002] Common quantum dots are a kind of compound semiconductor nanocrystals composed of II-VI or III-V elements, which can have various shapes such as spherical, polyhedral, and short rods, and can be stably dispersed in solvents. Between 1 and 10nm. Some quantum dots can produce fluorescence after being excited by light, and have excellent characteristics such as wide excitation spectrum range, narrow emission peak half-width, good space compatibility, and strong photobleaching resistance. Among the semiconductor quantum dots, the II-VI compound semiconductors are the most studied, and the research on CdSe quantum dots is the most thorough. Full coverage from blue light to red light and even near-infrared, and the emission wavelength is con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/02C09K11/88B82Y40/00
CPCB82Y40/00C09K11/02C09K11/883
Inventor 周一飞周海峰
Owner 周一飞