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A kind of preparation method of lead sulfide quantum dot fluorescent powder

A technology of quantum dots and lead sulfide, which is applied in the field of preparation of lead sulfide quantum dot phosphors, can solve the problems of incomplete preparation method of near-infrared quantum dots, incomplete research of near-infrared quantum dots, etc.

Active Publication Date: 2022-03-25
SHENZHEN PLANCK INNOVATION TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, quantum dot phosphors are mainly used in the production of white light LEDs. The research on the application of near-infrared quantum dots is not comprehensive, and the preparation method of near-infrared quantum dots is not perfect enough.

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  • A kind of preparation method of lead sulfide quantum dot fluorescent powder
  • A kind of preparation method of lead sulfide quantum dot fluorescent powder
  • A kind of preparation method of lead sulfide quantum dot fluorescent powder

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preparation example Construction

[0035] The specific embodiment of the present invention partially provides a preparation method of lead sulfide quantum dot phosphor, and the preparation method includes the following steps:

[0036] The lead source compound is mixed with an organic ligand and a solvent, heated and reacted under a protective gas atmosphere, and the temperature is lowered after the reaction is completed to obtain a lead precursor;

[0037] The solution containing the lead precursor is heated to the reaction temperature, and a sulfur source compound is added, and after the reaction is completed, the temperature is lowered, purified and dried to obtain the lead sulfide quantum dot phosphor.

[0038] In the present invention, the reaction principle of the lead precursor (taking PbO as an example) is:

[0039] Reaction formula:

[0040] The reaction principle of lead precursor (take PbO as an example) and sulfur precursor (take TMS as an example) is as follows:

[0041] Reaction formula:

[00...

Embodiment 1

[0053] Preparation of lead precursor:

[0054] In a 250ml three-necked flask, add PbO, OA, and ODE, and stir vigorously;

[0055]

[0056] Evacuate to make the vacuum degree below 200mTorr, switch to the Ar-filled state, repeat this step at least twice, and finally adjust to the Ar-filled state;

[0057] Gradually heat up to 150°C to prepare lead precursor, the color of the reactant gradually changes from yellow (color of PbO) to clear and transparent (color of lead oleate), and keep at 150°C for 10 minutes to make PbO and OA fully react, and then put The temperature drops to 110℃;

[0058] Continue to evacuate for 90 minutes, the degree of vacuum drops below 40mTorr, fill with Ar, the temperature will rise, and when the temperature drops back to 110 °C, continue to evacuate for 10 minutes, switch to the state of Ar filling, and heat up to the target temperature, wait for the temperature to stabilize, prepare ice bath conditions;

[0059] Prepare the sulfur precursor and...

Embodiment 2

[0072] Preparation of lead precursor:

[0073] In a 250ml three-necked flask, add PbO, OA, and ODE, and stir vigorously;

[0074]

[0075] Evacuate to make the vacuum degree below 200mTorr, switch to the Ar-filled state, repeat this step at least twice, and finally adjust to the Ar-filled state;

[0076] Gradually heat up to 140°C to prepare lead precursor, the color of the reactant gradually changes from yellow (color of PbO) to clear and transparent (color of lead oleate), and keep at 140°C for 20 minutes to make PbO and OA fully react. temperature drops to 100°C;

[0077] Continue to evacuate for 90 minutes, the degree of vacuum drops below 40mTorr, fill with Ar, the temperature will rise, wait for the temperature to drop back to 100 ℃, continue to evacuate for 10 minutes, switch to Ar filling state, heat up to 150 ℃, wait for its temperature to stabilize, prepare ice bath conditions;

[0078] Prepare the sulfur precursor and inject the reaction:

[0079] Use a syrin...

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Abstract

The invention provides a preparation method of lead sulfide quantum dot fluorescent powder. The preparation method comprises the following steps: mixing a lead source compound with an organic ligand and a solvent, heating and reacting under a protective gas atmosphere, and cooling down after the reaction to obtain Lead precursor: heating the solution containing the lead precursor to the reaction temperature, adding a sulfur source compound, cooling down after the reaction, purifying, and drying to obtain the lead sulfide quantum dot fluorescent powder. The preparation method can prepare PbS quantum dots with uniform particle size, the fluorescence quantum yield of quantum dots is less dependent on the wavelength of excitation light, and the QY value of quantum dots dispersed in tetrachlorethylene (TCE) solution is about 72%. Processed into powder QY value is about 45%.

Description

technical field [0001] The invention belongs to the field of quantum dots, and relates to a preparation method of quantum dot fluorescent powder, in particular to a preparation method of lead sulfide quantum dot fluorescent powder. Background technique [0002] Quantum dots, also known as semiconductor nanocrystals, were first used by Yale University physicist Reed in the late 1980s as a term to describe semiconductor crystals with very small three-dimensional dimensions. Today, quantum dots are defined as quasi-zero-dimensional materials with three-dimensional scales ranging from 1 to 100 nm. The size and shape of quantum dots can be precisely controlled by regulating the growth time, reaction temperature, and ligands of quantum dots. The size tunability of quantum dots is mainly due to two reasons. One is that the surface atoms of the nanocrystal are only a small fraction of the total number of atoms in the nanocrystal. The second is the structure of the quantum dot itse...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G21/21C09K11/66
Inventor 孙小卫王恺赵俊亮刘皓宸刘乙樽徐冰
Owner SHENZHEN PLANCK INNOVATION TECH CO LTD