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Preparation method of CuInS2/ZnS core-shell structure quantum dot and CuInS2/CdS/ZnS core-shell structure quantum dot

A core-shell structure and quantum dot technology is applied in the field of preparation of semiconductor nanomaterials, which can solve the problems of low quantum yield, blue shift of fluorescence emission spectrum, low fluorescence efficiency of quantum dots, etc. The effect of good performance and low equipment requirements

Active Publication Date: 2015-05-13
GUANGDONG POLY OPTOELECTRONICS
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Problems solved by technology

[0003] CuInS currently obtained by general technical means 2 The fluorescence efficiency of quantum dots is generally low, generally less than 5%.
In order to further improve the CuInS 2 The fluorescence efficiency of quantum dots can enhance their photochemical stability. At present, the more mature technology is to use continuous ion adsorption method on CuInS 2 ZnS inorganic shell layer is grown on the surface of quantum dots, but CuInS synthesized by existing technology 2 The fluorescence efficiency of ZnS quantum dots still cannot exceed 50%
Moreover, ZnS wrapped CuInS obtained by this method 2 After quantum dots, it will cause a blue shift in the fluorescence emission spectrum, and the quantum yield in the red and infrared regions is low, which cannot meet the requirements of CuInS 2 Applications of quantum dots in anti-counterfeiting, LED and biological detection

Method used

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  • Preparation method of CuInS2/ZnS core-shell structure quantum dot and CuInS2/CdS/ZnS core-shell structure quantum dot
  • Preparation method of CuInS2/ZnS core-shell structure quantum dot and CuInS2/CdS/ZnS core-shell structure quantum dot
  • Preparation method of CuInS2/ZnS core-shell structure quantum dot and CuInS2/CdS/ZnS core-shell structure quantum dot

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preparation example Construction

[0041] Such as Figure 1 to Figure 7 As shown, CuInS 2 The preparation method of / ZnS core-shell structure quantum dot comprises the following steps:

[0042] (1) Dissolve the copper source and indium source in the ratio of specific substances in the sulfur source, under the protection of nitrogen, heat to 120°C, keep warm until the solid particles are completely dissolved, and obtain the copper indium precursor liquid; continue to heat up to 220°C °C and incubated for 10-25 minutes to obtain CuInS with different particle sizes and fluorescence characteristics 2 Quantum dot solution;

[0043] (2) The CuInS obtained in step (1) 2 CuInS was obtained after the quantum dot solution was purified by centrifugation 2 quantum dots, will result in CuInS 2 Quantum dots are dispersed in octadecene and then heated to 230°C, zinc and sulfur precursor solutions are added dropwise within 20 to 30 minutes, and then incubated for 30 minutes to obtain CuInS 2 / ZnS core-shell quantum dot so...

Embodiment 1

[0051] Dodecanethiol was used as the sulfur source and solvent.

[0052] Preparation of zinc and sulfur precursor liquid: Disperse 4.8 mmol of zinc dibutyldithiocarbamate in 10 ml of octadecene solution and 4.8 mmol of sulfur powder into 15 ml of tributylphosphine.

[0053] Preparation of copper indium precursor liquid: 2.4mmol cuprous iodide, 2.4mmol indium acetate, and 30ml dodecanethiol were placed in a three-necked flask, heated to 120°C under the protection of nitrogen, and kept warm until the solid particles were completely dissolved.

[0054] CuInS 2 Preparation of quantum dots: Under the protection of nitrogen, the copper indium precursor solution was heated up to 220°C and reacted for 20 minutes to prepare CuInS 2 Quantum dot solution.

[0055] CuInS 2 Preparation of / ZnS core-shell quantum dots: CuInS obtained above 2 After the quantum dot solution was purified by centrifugation, CuInS 2 quantum dots, will result in CuInS 2 Quantum dots were dispersed into 30ml...

Embodiment 2

[0058] Octadecanol was used as the sulfur source and solvent.

[0059] Preparation of zinc and sulfur precursor liquid: Disperse 4.8 mmol of zinc diethyldithiocarbamate in 10 ml of octadecene and 4.8 mmol of sulfur powder into 15 ml of tributylphosphine.

[0060] Preparation of copper indium precursor liquid: disperse 2.4mmol cuprous iodide and 2.4mmol indium acetate in 30ml octadecyl mercaptan, place in a three-necked flask, heat to 120°C under the protection of nitrogen, and keep warm until the solid particles are completely dissolve.

[0061] CuInS 2 Preparation of quantum dots: under the protection of nitrogen, continue to heat up to 220 ° C, react for 25 minutes, and prepare CuInS 2 Quantum dot solution.

[0062] CuInS 2 Preparation of / ZnS core-shell quantum dots: CuInS obtained above 2 After the quantum dot solution was purified by centrifugation, CuInS 2 quantum dots, will result in CuInS 2 Quantum dots were dispersed into 30ml of octadecene, heated to 230°C aft...

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Abstract

The invention relates to a preparation method of a CuInS2 / ZnS core-shell structure quantum dot and a CuInS2 / CdS / ZnS core-shell structure quantum dot. The method comprises a preparation method of a CuInS2 multilayer core-shell structure quantum dot by using CuInS2 nano particles as follows: (1) dissolving a copper source and an indium source with a sulphur source to obtain a CuInS2 quantum dot solution; (2) centrifugally purifying the quantum dot solution; dropwise adding zinc and a sulphur precursor liquid to obtain a CuInS2 / ZnS core-shell structure quantum dot solution; and (3) dropwise adding the sulphur source and the sulphur precursor liquid into the CuInS2 quantum dot solution, and dropwise adding zinc and sulphur precursor liquid to obtain a CuInS2 / CdS / ZnS-type quantum dot. The preparation method is easy to operate, low in requirement on equipment and high in repeatability; and finally, the fluorescence quantum yield of the quantum dot is more than 50 percent, and a fluorescence-emission peak can be regulated in spectral ranges of visible light and infrared rays.

Description

technical field [0001] The invention relates to the technical field of preparation of semiconductor nanomaterials, in particular to CuInS 2 Preparation method of / ZnS core-shell quantum dots and CuInS 2 / CdS / ZnS core-shell structure quantum dots preparation method. Background technique [0002] Quantum dots, also known as semiconductor nanocrystals, have a particle physical diameter smaller than or close to the exciton Bohr radius. Due to the quantum size effect, quantum dots have a wide range of excitation wavelengths, narrow emission peaks and Gaussian symmetry, no tailing, Stokes It has the advantages of large Stein shift and strong photochemical stability. When stimulated by light or electricity, quantum dots will emit light in a certain wavelength range. The range and intensity of the emission spectrum are determined by the composition of quantum dots, their size and shape, and the modification of the particle surface. The unique photophysical and photochemical prope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/62
Inventor 谷小许李阳
Owner GUANGDONG POLY OPTOELECTRONICS
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