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Preparation method of novel high-efficient luminescence Mn-doped quantum dots

A quantum dot, high-efficiency technology, applied in the field of preparation of new high-efficiency luminescent Mn-doped quantum dots, can solve the problems of short fluorescence lifetime and limited space, and achieve the effects of low pollution, small production and use hazards, and excellent thermal stability

Active Publication Date: 2015-04-29
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the long fluorescence lifetime of this kind of Mn-doped quantum dots, it can effectively remove the interference of background signals in biological imaging applications, while the fluorescence lifetimes of Mn-doped quantum dots reported so far are all shorter than 2.5ms
In addition, these quantum dots contain heavy metal elements such as Cd and Se, which severely limit the space for their practical application.

Method used

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  • Preparation method of novel high-efficient luminescence Mn-doped quantum dots
  • Preparation method of novel high-efficient luminescence Mn-doped quantum dots
  • Preparation method of novel high-efficient luminescence Mn-doped quantum dots

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preparation example Construction

[0039] The preparation method of the novel high-efficiency luminescent Mn-doped quantum dot disclosed by the present invention comprises the following steps:

[0040] 1) Preparation of S precursor solution: Weigh an appropriate amount of sulfur powder and mercaptan or organic amine ligands (such as octadecylamine, dodecylamine, octaamine) and heat them at high temperature under an inert gas atmosphere to completely dissolve them in In octadecane, a transparent oil phase solution is formed;

[0041] 2) Preparation of Zn precursor solution: Mix an appropriate amount of Zn salt with ODE and organic amine ligands into a 10mL glass bottle, stir magnetically under an inert gas atmosphere and heat up to 50-70°C to form a transparent solution;

[0042] 3) Mix appropriate amount of manganese salt (0.05mmol), indium salt (0.2mmol), zinc salt (0.2mmol) with appropriate amount of octadecene (5mL), appropriate amount of n-dodecanethiol (1mL, DDT) and appropriate amount of oleylamine ( ...

Embodiment 1

[0056] In this embodiment, the inert gas atmosphere is an argon atmosphere.

[0057] Weigh 0.009g (0.05mmol) manganese acetate, 0.044g (0.2mmol) indium chloride, 0.036g (0.2mmol) zinc acetate, then add 1mL n-dodecanethiol (DDT) and 1mL oleylamine (OLA), 5mL Octadecane (ODE) was added to a 100mL three-necked bottle (the high-purity argon atmosphere in the bottle was ensured by repeated vacuuming and then argon). The temperature was raised from room temperature to 100° C. for 20 minutes to remove residual water molecules and low-boiling organic matter, and a transparent solution was obtained. Then the temperature was raised to 190°C.

[0058] Measure the sulfur (S) precursor solution (including 0.2mmol S powder, 1mL ODE and 1mL oleylamine (OLA), heat and dissolve into a transparent oil phase solution in an inert gas atmosphere) and quickly inject it into the three-necked bottle, and keep growing at the injection temperature After 30 minutes, Mn:Zn-In-S quantum dot crystal nucl...

Embodiment 2

[0061] In this embodiment, the inert gas atmosphere is a helium environment.

[0062] Weigh 0.009g (0.05mmol) manganese acetate, 0.044g (0.2mmol) indium chloride, 0.036g (0.2mmol) zinc acetate, then add 1mL n-dodecanethiol (DDT) and 1mL oleylamine (OLA), 5mL ODE was added to a 100mL three-necked flask. The high-purity helium atmosphere in the bottle is ensured by repeated vacuuming and recirculation of helium. The temperature was raised from room temperature to 100° C. for 20 minutes to remove residual water molecules and low-boiling organic matter, and a transparent solution was obtained. Then the temperature was raised to 220°C.

[0063] Measure a certain amount of sulfur (S) precursor solution (including 0.1mmol S powder, 1mL ODE and 1mL oleylamine (OLA), heat and dissolve into a transparent oil phase solution under an inert gas atmosphere) and quickly inject it into the three-necked bottle. The growth was maintained for 30 minutes to obtain Mn:Zn-In-S quantum dot crysta...

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Abstract

The invention discloses a preparation method of novel high-efficient luminescence Mn-doped quantum dots. The method comprises the following steps: adding powdered sulfur to 1-octadecene, and mixing to obtain a sulfur pecursor solution; adding Zn salt, In salt, a dopant Mn salt and an organic coating agent to the 1-octadecene, and heating to obtain a transparent solution; and heating the transparent solution under a protective gas, mixing with the sulfur pecursor solution, and reacting to obtain Mn:Zn-In-S bared quantum dots. ZnS shell layers wrap the surfaces Mn:Zn-In-S bared quantum dots obtained by the method; the optical property of the quantum dots can be effectively improved; and the fluorescent lifetime of the quantum dots can be prolonged. The synthesis condition provided by the invention is simple, safe, and uniform in particle size distribution, does not contain heavy metal elements such as Cd and Se; the fluorescence quantum efficiencies are 56%; the fluorescent lifetime is 4.8ms; and the Mn-doped quantum dots obtained by the method have excellent heat-resistant stability, can bear hot weather fastness of 200 DEG C, and show an attractive application prospect in the aspects such as photoelectronic devices and biological fluorescence labels.

Description

technical field [0001] The invention relates to a method for preparing quantum dots, in particular to a method for preparing novel high-efficiency luminescent Mn-doped quantum dots. Background technique [0002] When the size of the material is reduced to the nanometer level, due to its nano-effect, the material will produce many novel and unique functional properties superior to traditional materials, and has potential in the fields of microelectronics, bioengineering, fine ceramics, chemical industry, and medicine. wide application. [0003] In recent years, nano-luminescent materials with transition metals as active ions have attracted the attention of many scholars at home and abroad due to their excellent optical properties. It has been found that the optical, electrical, magnetic and other properties of nanomaterials can be greatly improved and enhanced by proper doping. Group II-VI semiconductors are semiconductors with wide bandgap. The optical properties can be a...

Claims

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Application Information

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IPC IPC(8): C09K11/62
Inventor 郑金桔曹盛王霖高凤梅尉国栋尚明辉杨祚宝杨为佑
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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