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Preparation method for quaternary ZnCuInS3 quantum dot with high fluorescence

A fluorescent performance and quantum dot technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of large nanocrystal size, no fluorescent properties, narrow wavelength adjustment range, etc., achieve high quantum yield, improve luminous efficiency, The effect of easy operation

Inactive Publication Date: 2012-09-19
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The introduction of zinc can improve the luminous efficiency (5%). By adjusting the particle size and zinc content, the fluorescence emission range can be adjusted from 570nm to about 800nm, but the wavelength adjustment range is narrow
In 2007, Lu's group synthesized sphalerite CuInS for the first time by thermal injection method. 2 , and Zn was introduced into it to obtain quaternary Zn-Cu-In-S nanocrystals with adjustable bandgap structure, but due to the large size of the obtained nanocrystals, there is no fluorescent property

Method used

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  • Preparation method for quaternary ZnCuInS3 quantum dot with high fluorescence
  • Preparation method for quaternary ZnCuInS3 quantum dot with high fluorescence
  • Preparation method for quaternary ZnCuInS3 quantum dot with high fluorescence

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Weigh 29.2mg (0.1mmol) In(Ac) 3 , 19.1mg (0.1mmol) CuI, 21.9mg (0.1mmol) Zn(Ac) 2 In a 25ml four-neck flask, add 482ul (2mmol) dodecyl mercaptan, 126ul (0.4mmol) oleic acid, 5ml octadecene, and heat under the condition of first vacuuming and then backfilling with argon to obtain Zn 2+ 、Cu + 、In 3+ Cation precursor solution: Weigh 38.4mg (1.2mmol) of elemental S into a single-mouth round bottom bottle, add 4ml (12mmol) of oleylamine, 2ml of octadecene, and ultrasonically dissolve to obtain a clear S precursor solution.

[0036] 2) Under the protection of argon, the Zn 2+ 、Cu + 、In 3+ The cation precursor solution was quickly injected into the S precursor solution under the condition of 180°C, and after reacting for 15 minutes, the heat source was removed and cooled to room temperature, and the quaternary ZnCuInS was obtained by centrifugal purification. 3 quantum dots;

[0037] Such as figure 1 , for the resulting quaternary ZnCuInS 3 Quantum dots were tested...

Embodiment 2

[0039] 1) Weigh 44.2mg (0.2mmol) InCl 3 , 19.1mg (0.1mmol) CuI, 63.2mg (0.1mmol) Zn(SA) 2 In a 25ml four-neck flask, add 1.26ml (5.3mmol) dodecyl mercaptan, 350ul (1.1mmol) oleic acid, 8ml octadecene, under the condition of first vacuuming and then backfilling with argon protection Heating to get Zn 2+ 、Cu + 、In 3+ Cation precursor solution: Weigh 38.4mg (1.2mmol) of elemental S into a single-mouth round bottom bottle, add 4ml (12mmol) of oleylamine, 2ml of octadecene, and ultrasonically dissolve to obtain a clear S precursor solution.

[0040] 2) Under the protection of argon, the Zn 2+ 、Cu + 、In 3+ The cation precursor solution was rapidly heated to 210°C, injected into the S precursor solution, and reacted for 20 minutes, then removed the heat source and cooled to room temperature, and purified by centrifugation to obtain quaternary ZnCuInS 3 quantum dots;

[0041] Such as figure 2 , for the resulting quaternary ZnCuInS 3 Quantum dots were tested by ultraviolet a...

Embodiment 3

[0043] 1) Weigh 87.6mg (0.3mmol) In(Ac) 3 , 12.3mg (0.1mmol) CuAc, 63.2mg (0.1mmol) Zn(SA) 2 In a 25ml four-neck flask, add 1.19ml (5mmol) of dodecyl mercaptan, 320ul (1mmol) of oleic acid, 10ml of octadecene, and heat under the condition of first vacuuming and then backfilling with argon to obtain Zn 2+ 、Cu + 、In 3+ Cation precursor solution: Weigh 32mg (1mmol) of elemental S into a single-mouth round bottom bottle, add 3.3ml (10mmol) of oleylamine, 1.7ml of octadecene, and ultrasonically dissolve to obtain a clear S precursor solution.

[0044] 2) Under the protection of argon, the Zn 2+ 、Cu + 、In 3+ The cation precursor solution was rapidly heated to 240°C, injected into the S precursor solution, reacted for 30 minutes, removed the heat source and cooled to room temperature, and purified by centrifugation to obtain quaternary ZnCuInS 3 quantum dots;

[0045] Such as image 3 , for the resulting quaternary ZnCuInS 3 Quantum dots were tested by ultraviolet absorptio...

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Abstract

The invention relates to a preparation method for quaternary ZnCuInS3 with the high fluorescence, which comprises the following steps of: firstly, preparing precursor solution of Zn<2+>, Cu<+> and In<3+> cations; under the protection of argon, quickly heating the precursor solution to 180-240DEG C from the room temperature; quickly injecting S precursor solution to react for 15-30 minutes; removing a heat source, and naturally cooling to the room temperature; and centrifuging and purifying to obtain the quaternary ZnCuInS3 quantum dot. The obtained quaternary ZnCuInS3 quantum dot has good fluorescence, the fluorescence emission peak position of the quaternary ZnCuInS3 quantum dot is within the range of 645-825nm, and the fluorescence quantum dot productivity is 55-64%. According to the preparation method disclosed by the invention, cheap and nontoxic precursor material is adopted and is synthesized into the quaternary ZnCuInS3 quantum dot with the high fluorescence with a simple thermal injection method, wherein the wavelength of the quaternary ZnCuInS3 quantum dot is 825nm, the quaternary ZnCuInS3 quantum dot can carry out near-infrared luminescence, and the fluorescence quantum dot productivity of the quaternary ZnCuInS3 quantum dot is 55-64%. A foundation is laid for applying the quantum dot to living body bioimaging.

Description

technical field [0001] The invention relates to the technical field of preparation of compound semiconductor nanomaterials, in particular to a quaternary ZnCuInS with high fluorescence performance 3 Preparation methods of quantum dots. Background technique [0002] Quantum dots (QDs) are inorganic semiconductor light-emitting nanocrystals. Due to their unique quantum effects and optical properties, they have broad development space in the detection fields of cell imaging, molecular imprinting, and living organism labeling. [0003] The current mainstream Ⅱ-Ⅵ and Ⅲ-Ⅴ semiconductor nanocrystals have achieved great success in synthesis and optical property regulation, but some defects in binary quantum dots make their application prospects very slim. For example, the composition of A-type elements (Cd, Pb, Hg) and B-type elements (P, Te, As) limits its market and application range; some high-cost, high-risk components required in the quantum dot synthesis process Reagents (su...

Claims

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Application Information

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IPC IPC(8): C09K11/62
Inventor 常津董春红郭伟圣
Owner TIANJIN UNIV
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