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Synthesis method of platy-ZnSe fluorescent nano monocrystal

A fluorescent nano-synthesis method, applied in the field of synthesis of nano-materials, can solve the problems of preparation of flaky ZnSe nano-single crystals, long photodegradation time, and difficulty in washing nano-crystals.

Inactive Publication Date: 2010-07-28
YUNNAN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

(2) Chinese patent 200610024520.1 uses aqueous medium to synthesize ZnSe / ZnS core-shell quantum dots, which requires a long photodegradation time in the process of preparing quantum dots
[0005] In short, there are still deficiencies in the current synthesis process of ZnSe nanocrystals: 1. No matter whether the current synthesis method is in the aqueous phase or in the organic phase, there is no report to prepare flaky ZnSe nano single crystals with luminescent properties.
However, the introduction of long-chain alkanes (such as tetradecane) makes the washing of nanocrystals very difficult.

Method used

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  • Synthesis method of platy-ZnSe fluorescent nano monocrystal
  • Synthesis method of platy-ZnSe fluorescent nano monocrystal

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Experimental program
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Embodiment 1

[0047] Synthesis of flaky ZnSe fluorescent nano single crystals:

[0048] 1. First, heat 0.6 mmol of selenium and 1 g of trioctylphosphine in an oil bath at 40° C. under the protection of nitrogen, and stir for one hour to obtain a selenium precursor.

[0049] 2. Stir and mix 2 g of octadecene, 0.085 mmol of zinc stearate, and 0.4 mmol of octadecylamine under the protection of nitrogen to obtain a zinc precursor. The zinc precursor was "activated" by stirring at 50°C for 3 hours.

[0050] 3. Add 8 mmol of octadecyl mercaptan to the zinc precursor under nitrogen protection, and then stir at 50° C. for 1 hour to perform “template” treatment.

[0051] 4. Continue to raise the temperature of the zinc precursor system to 305°C under the protection of nitrogen, and quickly inject the selenium precursor into the zinc precursor while stirring. At this time, the temperature of the reaction system drops to 275°C, and the nanocrystals begin to grow, and the reaction start the timer.

...

Embodiment 2

[0055] 1. Firstly, 0.6 mmol of selenium and 1 g of trioctylphosphine were heated at 40° C. under the protection of argon and ultrasonicated for half an hour to obtain a selenium precursor.

[0056] 2. Stir and mix 2 g of octadecene, 0.1 mmol of zinc stearate, and 0.8 mmol of octadecylamine under the protection of argon to obtain a zinc precursor. The zinc precursor was "activated" by ultrasonication at 70°C for 1 hour.

[0057] 3. Add 8 mmol of octadecyl mercaptan to the zinc precursor under nitrogen protection, and then stir at 65° C. for 0.5 hour to perform “template” treatment.

[0058] 4. Continue to raise the temperature of the zinc precursor system to 305°C under the protection of argon, and quickly inject the selenium precursor into the zinc precursor while stirring. At this time, the temperature of the reaction system drops to 275°C, and the nanocrystals begin to grow. The reaction starts timing.

[0059] 5. After the nanocrystals start to grow, when the reaction tim...

Embodiment 3

[0062] 1. First, 0.6 mmol of selenium and 1 g of trioctylphosphine were heated at 40° C. under nitrogen protection and ultrasonicated for half an hour to obtain a selenium precursor.

[0063] 2. Fully grind the zinc precursor composed of 2 g of octadecene, 0.085 mmol of zinc stearate, and 0.8 mmol of hexadecylamine at 25° C. for 3 hours to realize its “activation” treatment.

[0064] 3. Add 4 mmol of octadecyl mercaptan to the zinc precursor under nitrogen protection, and then stir at 70° C. for 1 hour to perform “template” treatment.

[0065] 4. Under the protection of nitrogen, raise the temperature of the zinc precursor system to 315°C, quickly inject the selenium precursor into the zinc precursor while stirring, at this time, the temperature of the reaction system drops to 290°C, the nanocrystals begin to grow, and the reaction start the timer.

[0066] 5. After the nanocrystals start to grow, when the reaction time reaches 1 hour and 30 minutes, stop heating and end the ...

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Abstract

The invention belongs to a synthesis method of nano material, in particular to a synthesis method of platy-ZnSe fluorescent nano monocrystal, which comprises: under inert gas protection, heating and stirring or ultra-dissolving elementary substance Se in trioctylphosphine to obtain Se precursor; dissolving Zn source in octadecene, and adding activator long-chain alkylamines under inert gas protection to carry out 'activation' treatment; then introducing template agent long-chain alkyl sulfhydryl to carry out 'templated' treatment to activated Zn precursor, and finally heating up to the synthesis reaction temperature (300 to 350 DEG C) under inert gas protection; quickly adding the Se precursor in the Zn precursor, and reacting for a certain time to obtain original solution crude product of the platy-ZnSe fluorescent nano monocrystal. The final product of clear solvent of platy-ZnSe fluorescent nano monocrystal can be obtained through adding mixed solution consisting of high-polar organic solvent and low-polar organic solvent to wash and centrifuge, and finally dissolving with the low-polar organic solvent. The method has the advantages of simple reaction system, easy availability of raw material, little environment pollution, good crystallinity and high fluorescent quantum yield.

Description

technical field [0001] The invention relates to a method for synthesizing nanometer materials. In an organic phase reaction environment, a surface active agent is used as a template, and the "template" treatment of Zn precursor is adopted to realize the synthesis of flake ZnSe fluorescent nanometer single crystal. Background technique [0002] Zinc selenide (ZnSe) nanocrystals are an important direct wide-bandgap II-VI semiconductor luminescent material with different physical, chemical and optical properties than bulk materials. Because of its unique photoelectric properties, it has extremely broad application prospects in the fields of biological probes, short-wavelength optoelectronic devices, spintronics, solar cells, infrared and terahertz emission, etc. [0003] At present, the synthesis routes of ZnSe semiconductor nanocrystals can be mainly divided into aqueous phase synthesis and organic phase synthesis according to the reaction medium. Among them, the synthesis re...

Claims

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Application Information

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IPC IPC(8): C30B29/48C30B29/64C30B7/14C09K11/88
Inventor 蒋峰芝李艳娟
Owner YUNNAN UNIV
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