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Method for preparing chalcopyrite structure CuInSe2 or/and CuInSe2/ZnS core-shell structure quantum dots

A core-shell structure and quantum dot technology, which is applied in the field of compound semiconductor nanomaterial preparation, can solve the problems of quantum dot application limitation, expensive raw material price, and fluorescence quantum yield less than 5%, avoiding the use of precursor raw materials and simplifying the preparation. Process and the effect of mass production

Inactive Publication Date: 2012-09-12
TIANJIN UNIV
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Problems solved by technology

Nose et al synthesized CuInSe with emission wavelength in the range of 820-940nm 2 Quantum dots, but the fluorescence quantum yield is less than 5%; and Cassette et al. studied the synthesis of CuInSe by using selenourea as the precursor of selenium in one pot 2 and CuInSe 2 / ZnS core / shell quantum dots, the emission wavelength is in the range of 700-1000nm, and the quantum yield of quantum dots with fluorescence emission of 800nm ​​after ZnS coating is increased to 40-50%
Although the fluorescence yield of quantum dots has increased, the application of quantum dots has been limited due to their expensive raw material prices.

Method used

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  • Method for preparing chalcopyrite structure CuInSe2 or/and CuInSe2/ZnS core-shell structure quantum dots
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  • Method for preparing chalcopyrite structure CuInSe2 or/and CuInSe2/ZnS core-shell structure quantum dots

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Weigh 29.2mg (0.1mmol) In(Ac) 3 , 9.9mg (0.1mmol) CuCl in a 25ml four-neck flask, and add 1.39ml (8mmol) n-octyl mercaptan, 6ml of octadecene, magnetic stirring for 30min under vacuum conditions, until the cationic precursor liquid is completely dissolved to To clarify, get Cu + 、In 3+ Cation precursor solution: Weigh 31.6mg (0.4mmol) of elemental Se in a single-mouth round bottom bottle, add 536ul (1.2mmol) of TOP, 2ml of octadecene, dissolve until clear to obtain Se precursor solution.

[0040] 2) Backfill the system with argon, and the Cu + 、In 3+ The cation precursor solution was rapidly heated from room temperature to 230°C, injected into the Se precursor solution, reacted for 45 minutes, removed the heat source, cooled to room temperature, and centrifuged to obtain CuInSe 2 quantum dots;

[0041] Such as figure 1 As shown, the obtained CuInSe 2 The XRD spectrum of quantum dots proves that the obtained nanocrystals are chalcopyrite structures; as figure...

Embodiment 2

[0043] 1) Weigh 44.2mg (0.2mmol) In(Cl) 3 , 19.1mg (0.1mmol) CuI in a 25ml four-neck flask, and add 1.43ml (6mmol) dodecyl mercaptan, 8ml of octadecene, magnetic stirring for 30min under vacuum conditions, until the cationic precursor liquid is completely Dissolve until clear to give Cu + 、In 3+ Cation precursor solution: Weigh 47.4mg (0.6mmol) of elemental Se into a single-mouth round bottom bottle, add 450ul (1.8mmol) of TBP and 3ml of octadecene, dissolve until clear to obtain Se precursor solution.

[0044] 2) Backfill the system with argon, and the Cu + 、In 3+ The cation precursor solution was rapidly heated from room temperature to 200°C, injected into the Se precursor solution, reacted for 15 minutes, removed the heat source, cooled to room temperature, and centrifuged to obtain CuInSe 2 quantum dots;

[0045] Such as figure 1 As shown, the obtained CuInSe 2 The XRD spectrum of quantum dots proves that the obtained nanocrystals are chalcopyrite structures; as f...

Embodiment 3

[0047] 1) Weigh 148.7mg (0.3mmol) InI 3 , 12.3mg (0.1mmol) CuAc in a 25ml four-neck flask, and add 1.35ml (4mmol) octadecyl mercaptan, 7ml of octadecene, magnetic stirring under vacuum conditions for 30min, until the cationic precursor liquid is completely Dissolve until clear to give Cu + 、In 3+ Cation precursor solution: Weigh 632mg (0.8mmol) of elemental Se in a single-mouth round bottom bottle, add 600ul (2.4mmol) of TBP and 4ml of octadecene, and dissolve until clarified to obtain Se precursor solution.

[0048] 2) Backfill the system with argon, and the Cu + 、In 3+ The cation precursor solution was rapidly heated from room temperature to 250 °C, injected into the Se precursor solution, reacted for 60 minutes, removed the heat source and cooled to room temperature, and centrifuged to obtain CuInSe 2 quantum dots;

[0049] Such as figure 1 As shown, the obtained CuInSe 2 The XRD spectrum of quantum dots proves that the obtained nanocrystals are chalcopyrite structur...

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Abstract

The invention relates to a method for preparing chalcopyrite structure CuInSe2 or / and CuInSe2 / ZnS core-shell structure quantum dots, comprising the following steps: firstly preparing an In3<+>, Cu<+> cation precursor solution, rapidly heating up from room temperature to 200-250 DEG C under the protection of argon, rapidly injecting an Se precursor solution, reacting for 15-60 min to obtain a CuInSe2 quantum dot solution; reacting for 30-60min at 190-230 DEG C by dropwisely adding a zinc precursor solution, then naturally cooling to room temperature, and carrying out centrifugal purification to obtain CuInSe2 / ZnS core-shell structure quantum dots, wherein the obtained CuInSe2 quantum dots have a chalcopyrite crystal structure, the atomic ratio of Cu to In to Se is close to 1 to 1 to 2, the range of the fluorescence emission peak of the CuInSe2 / ZnS core-shell structure quantum dots is 700-960 nm, and the fluorescence quantum yield is 19.8-33.4 %. According to the invention, the method uses the low-cost Se precursor, the process is simple, the synthetic period is short, the method is beneficial for batch production, and the synthesized CuInSe2 / ZnS quantum dots are near-infrared luminous and have good fluorescence efficiency, and lay the foundations for the application of quantum dots in bioluminescence imaging in vivo.

Description

technical field [0001] The invention relates to the technical field of preparation of compound semiconductor nanomaterials, in particular to a chalcopyrite structure CuInSe 2 and CuInSe 2 A preparation method of quantum dots with / ZnS core-shell structure. Background technique [0002] Quantum dots (QDs) are quasi-zero-dimensional nanomaterials, which are composed of a small number of atoms. The physical diameter of the particles is in the range of 1-10nm, which is smaller than or close to the exciton Bohr radius. Based on quantum effects, quantum dots have unique optical properties and are an inorganic semiconductor light-emitting nanocrystal. Compared with traditional organic fluoresceins, quantum dots have the advantages of wide excitation spectrum and continuous distribution, narrow emission peak and Gaussian symmetry, no tailing, large Stokes shift, strong photochemical stability, and long fluorescence lifetime. In addition, chemically modified quantum dots have good...

Claims

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Application Information

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IPC IPC(8): C09K11/88
Inventor 常津董春红郭伟圣
Owner TIANJIN UNIV
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