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 emis

Method used

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

Examples

Experimental program
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Effect test

Example Embodiment

[0038] Example 1:

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

[0040] 2) Backfill the system with argon, and add Cu + , In 3+ The cation precursor solution was quickly heated from room temperature to 230°C, and the Se precursor solution was injected. After 45 minutes of reaction, the heat source was removed and cooled to room temperature. CuInSe was purified by centrifugation. 2 Quantum dot

[0041] Such as figure 1 As shown, the obtained CuInSe 2 The XRD pattern of the quantum dots proves that the obtained nanocr...

Example Embodiment

[0042] Example 2:

[0043] 1) Weigh 44.2mg (0.2mmol) In(Cl) 3 , 19.1mg (0.1mmol) CuI in a 25ml four-necked flask, and add 1.43ml (6mmol) dodecyl mercaptan, 8ml of octadecene, magnetically stirred for 30min under vacuum, until the cationic precursor liquid is complete Dissolve to clear, get Cu + , In 3+ Cationic precursor solution: Weigh 47.4mg (0.6mmol) of elemental Se into a single-necked round bottom flask, add 450ul (1.8mmol) TBP, 3ml of octadecene, and dissolve it until clear to obtain a Se precursor solution.

[0044] 2) Backfill the system with argon, and add Cu + , In 3+ The cation precursor solution was quickly heated from room temperature to 200°C, and the Se precursor solution was injected. After 15 minutes of reaction, the heat source was removed and cooled to room temperature, and the CuInSe was purified by centrifugation. 2 Quantum dot

[0045] Such as figure 1 As shown, the obtained CuInSe 2 The XRD pattern of the quantum dots proves that the obtained nanocrystals are c...

Example Embodiment

[0046] Example 3:

[0047] 1) Weigh 148.7mg (0.3mmol) InI 3 , 12.3mg (0.1mmol) CuAc in a 25ml four-necked flask, and add 1.35ml (4mmol) octadecyl mercaptan, 7ml octadecene, magnetically stirred for 30min under vacuum, until the cationic precursor liquid is complete Dissolve to clear, get Cu + , In 3+ Cationic precursor solution: Weigh 632mg (0.8mmol) of elemental Se into a single-necked round-bottomed flask, and add 600ul (2.4mmol) TBP and 4ml of octadecene, and dissolve it until clear to obtain a Se precursor solution.

[0048] 2) Backfill the system with argon, and add Cu + , In 3+ The cation precursor solution was quickly heated from room temperature to 250°C, and the Se precursor solution was injected. After 60 minutes of reaction, the heat source was removed and cooled to room temperature. CuInSe was purified by centrifugation. 2 Quantum dot

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

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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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