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Method for preparing tetrahedral light-emitting indium phosphide/zinc sulfide core-casing quantum dots

A technology of core-shell structure and quantum dots, which is applied in the field of chemical synthesis of tetrahedral indium phosphide/zinc sulfide core-shell structure quantum dots, which can solve adverse reactions, safety control, controllable reactions, unstable raw materials, and raw material costs Advanced problems, to achieve the effect of ensuring fluorescence quantum yield, storage and use safety, mild reaction and safety

Active Publication Date: 2017-11-03
南京紫同纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] L. Li and P. Reiss, J. Am. Chem. Soc. 2008, 130, 11588-11589.) This method not only has high cost of raw materials, unstable raw materials, but also requires harsh reaction conditions
Although the use of (tris(diethylamino)phosphine) as a phosphorus source to prepare indium phosphide quantum dots has been developed in recent years, which can greatly reduce the cost of synthesis and the conditions of the reaction; however, the generation of a large amount of gas during the reaction is not Conducive to the safety control of the reaction, and the controllable regulation of the reaction

Method used

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  • Method for preparing tetrahedral light-emitting indium phosphide/zinc sulfide core-casing quantum dots
  • Method for preparing tetrahedral light-emitting indium phosphide/zinc sulfide core-casing quantum dots
  • Method for preparing tetrahedral light-emitting indium phosphide/zinc sulfide core-casing quantum dots

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Preparation of blue InP / ZnS core-shell quantum dots

[0040] (1) Mix 24 mmol tris(dimethylamino)phosphine and 60 mmol oleylamine at room temperature. The system was evacuated, stirred and heated to 80 o C, and maintain the reaction temperature for 30 min to obtain tris(dioleylamino)phosphine.

[0041] (2) Preparation of InCl 3 and ZnI 2 The oleylamine solution makes InCl 3 and ZnI 2 The concentrations are 0.068 and 0.440mol / L, respectively. The solution was stirred and heated to 150°C under vacuum o C, and maintain this temperature for 2 h.

[0042] (3) to the InCl 3 and ZnI 2 Inject inert gas in the reaction bottle of oleylamine solution, and system temperature is raised to 200 o C. Rapidly inject tris(dioleylamino)phosphine, and keep the molar ratio of indium halide to tris(dioleylamino)phosphine at 7:1, and maintain the temperature for 20 min.

[0043] (4) After preparing the InP quantum dot core, immediately inject the octadecene solution of n-...

Embodiment 2

[0050] Example 2: Preparation of green InP / ZnS core-shell quantum dots

[0051] (1) Mix 24 mmol tris(dimethylamino)phosphine and 60 mmol oleylamine at room temperature. The system was evacuated, stirred and heated to 80 o C, and maintain the reaction temperature for 30 min to obtain tris(dioleylamino)phosphine.

[0052] (2) Preparation of InCl 3 and ZnI 2 The oleylamine solution makes InCl 3 , ZnI 2and ZnCl 2 The concentrations are 0.068, 0.136 and 0.306mol / L, respectively. The solution was stirred and heated to 150°C under vacuum o C, and maintain this temperature for 2 h.

[0053] (3) to the InCl 3 and ZnI 2 Inject inert gas in the reaction bottle of oleylamine solution, and system temperature is raised to 200 o C. Rapidly inject tris(dioleylamino)phosphine, and keep the molar ratio of indium halide to tris(dioleylamino)phosphine at 7:1, and maintain the temperature for 20 min.

[0054] (4) After the InP quantum dot core is prepared, the octadecene solution of n-...

Embodiment 3

[0061] Example 3: Preparation of red InP / ZnS core-shell quantum dots

[0062] (1) Mix 24 mmol tris(dimethylamino)phosphine and 60 mmol oleylamine at room temperature. The system was evacuated, stirred and heated to 80 o C, and maintain the reaction temperature for 30 min to obtain tris(dioleylamino)phosphine.

[0063] (2) Preparation of InCl 3 and ZnI 2 The oleylamine solution makes InCl 3 , ZnCl 2 The concentrations are 0.068 and 0.440mol / L, respectively. The solution was stirred and heated to 150°C under vacuum o C, and maintain this temperature for 2 h.

[0064] (3) to the InCl 3 and ZnI 2 Inject inert gas in the reaction bottle of oleylamine solution, and system temperature is raised to 200 o C. Rapidly inject tris(dioleylamino)phosphine, and keep the molar ratio of indium halide to tris(dioleylamino)phosphine at 7:1, and maintain the temperature for 20 min.

[0065] (4) After the InP quantum dot core is prepared, the octadecene solution of n-dodecyl mercaptan a...

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Abstract

The invention discloses a method for preparing tetrahedral light-emitting indium phosphide / zinc sulfide core-casing quantum dots. The method comprises the following steps: preparing high-boiling point tris(dialiphatic amido) phosphine, preparing InP quantum dot cores, preparing InP / ZnS core-casing quantum dots and separating the InP / ZnS core-casing quantum dots. Through the use of the high-boiling point tris(dialiphatic amido) phosphine as a phosphorus source, the price is low, the chemical structure is stable, the reaction is mild and safe, and gas is not produced. All reaction precursors are common chemical reagents and low in toxin and safe to store and use. The luminescent color of the InP / ZnS core-casing quantum dots can be precisely controlled simultaneously by the reaction temperature, the ratio of indium halide to the tris(dialiphatic amido) phosphine, the type of the halide and the reaction time, and high fluorescence quantum yield can be ensured.

Description

technical field [0001] The invention relates to a synthesis method of quantum dots, in particular to a chemical synthesis method of regular tetrahedral shape indium phosphide / zinc sulfide core-shell structure quantum dots. Background technique [0002] Due to the low toxicity of the material, indium phosphide quantum dots play an important role in basic research and industrial production such as biomarkers, quantum dot luminescence and display. So far, common chemical synthesis methods for indium phosphide quantum dots usually use tris(trimethylsilyl)phosphine, which is relatively expensive and difficult to store, as the phosphorus source, fatty acid indium as the indium source, and liquid olefin as the solvent at 200 -300 o Indium phosphide was prepared under the conditions of C. (see [0003] L. Li and P. Reiss, J. Am. Chem. Soc. 2008, 130, 11588-11589.) This method not only has high cost of raw materials, unstable raw materials, but also requires harsh reaction conditi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/70
CPCC09K11/703
Inventor 邓正涛沈炜
Owner 南京紫同纳米科技有限公司
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