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Method for removing residual cationic precursors from oil-soluble quantum dots

A quantum dot and oil-soluble technology, applied in chemical instruments and methods, luminescent materials, etc., can solve problems affecting the purity of quantum dot solutions, the luminous efficiency and life of QLED devices, etc., to improve reproducibility, easy to repeat, and reproducible good control effect

Active Publication Date: 2016-10-12
TCL CORPORATION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for removing residual cationic precursors in oil-soluble quantum dots, aiming to solve the problem that residual cationic precursors in oil-soluble quantum dots affect the purity of quantum dot solutions, thereby affecting the luminous efficiency and life of QLED devices The problem

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  • Method for removing residual cationic precursors from oil-soluble quantum dots

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Embodiment 1

[0038] A Cd that removes blue luminescence x Zn 1-x The method for residual cationic precursor in S / ZnS oil-soluble quantum dots, comprises the following steps:

[0039] S11. Under the protection of Ar gas, take 20ml of Cd x Zn 1-x S / ZnS quantum dots (0.05mg / ml) n-hexane solution was injected into a three-necked flask containing 3ml of oleic acid (OA) and 3ml of octadecene (ODE) to obtain blue oil-soluble quantum dots with residual cationic precursors mixed solution;

[0040] S12. Heat the blue oil-soluble quantum dot mixture in the three-necked flask to 80°C and maintain it for 20 minutes, then raise the temperature to 180°C to make the blue oil-soluble quantum dot mixture become a clear liquid and maintain it for 30 minutes , then drop the temperature of the blue oil-soluble quantum dot mixture to 150° C. and then add oleylamine to obtain the first mixture, wherein the amount of oleylamine added satisfies: the molar ratio of the cationic precursor to the oleylamine 1:2;...

Embodiment 2

[0045] A Cd that removes red or green luminescence 1-x Zn x Se 1-y S y A method for residual cationic precursors in oil-soluble quantum dots, comprising the following steps:

[0046] S21. Under the protection of Ar gas, take 20ml of Cd 1-x Zn x Se 1-y S y Quantum dots (0.05mg / ml) n-hexane solution was injected into a three-necked flask containing 3ml of oleic acid (OA) and 3ml of octadecene (ODE), to obtain a blue oil-soluble quantum dot mixed solution of residual cation precursor;

[0047] S22. Heating the red or green luminescent oil-soluble quantum dot mixture in the three-necked flask to 80°C and maintaining it for 20 minutes, then raising the temperature to 180°C to make the red or green oil-soluble quantum dot mixture become a clear and transparent liquid and Maintain for 30 minutes, then lower the temperature of the red or green oil-soluble quantum dot mixture to 150°C and then add oleylamine to obtain the first mixture, wherein the amount of oleylamine added sat...

Embodiment 3

[0051] A method for directly removing residual cationic precursors in the reaction system to obtain high-purity oil-soluble quantum dots. This example is suitable for the system of using oleic acid and octadecene as reaction solvents to synthesize quantum dots. For the synthesis of quantum dots, refer to Chemistry of Materials 2008,20,5307-5313, its synthesis comprises the following steps:

[0052] S311. Preparation of zinc oleate and cadmium oleate mixture: 9 mmol of zinc acetate, 1 mmol of cadmium oxide, 8 mL of oleic acid, and 15 mL of octadecene were placed in a 50 mL three-necked flask. Degas at room temperature, heat up to 120°C for 20mins, pass argon and heat up to 120°C for 10mins, and finally heat the mixture to 250°C until a clear, transparent solution is formed.

[0053] S312. Preparation of S-ODE: 1.8 mmol of S was added to 3 ml of octadecene, heated to 230°C until a clear and transparent solution was formed, and then kept at 140°C.

[0054] S313. Preparation of S...

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Abstract

The invention provides a method for removing residual cationic precursors from oil-soluble quantum dots. The method includes steps: providing oil-soluble quantum dot mixed liquid with the residual cationic precursors; adding organic amine into the oil-soluble quantum dot mixed liquid under an air, inertia or vacuum atmosphere, and performing thermal mixing at a temperature of 80-350 DEG C to obtain first mixed liquid; cooling the first mixed liquid to 30-120 DEG C, and adding a nonpolar organic solvent to perform secondary mixing to obtain second mixed liquid; cooling the second mixed liquid to the room temperature, adding a polar organic solvent to form turbid liquid, and centrifuging the turbid liquid to obtain the oil-soluble quantum dots.

Description

technical field [0001] The invention belongs to the technical field of oil-soluble quantum dot purification, and in particular relates to a method for removing residual cation precursors in oil-soluble quantum dots. Background technique [0002] In recent years, due to the advantages of high light color purity, high luminous quantum efficiency, adjustable luminous color, and long service life, quantum dot light-emitting diodes (QLEDs) with quantum dot materials as the light-emitting layer have received extensive attention and become a new type of LED. main direction of research. With the development of QLED printing technology, QLED is most likely to become the product of printing display in the future. For printing and preparing QLED devices, a high-purity red, green and blue quantum dot solution is necessary. However, the luminous efficiency and lifetime of blue quantum dot light-emitting diodes are far from meeting the display requirements, which has become a key factor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/56C09K11/88C09K11/70C09K11/62
CPCC09K11/565C09K11/621C09K11/70C09K11/883
Inventor 刘政程陆玲聂志文覃辉军杨一行曹蔚然钱磊
Owner TCL CORPORATION
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