Method for synthesizing bar-shaped ZnSe fluorescence nanocrystalline

A technology of fluorescent nanocrystals and synthesis methods, applied in the field of nanomaterial synthesis, can solve the problems of long photodegradation time, nanocrystal surface defects, non-dense crystals, etc., and achieve high fluorescence quantum yield, toxicity and cost reduction, simplification The effect of the reaction system

Inactive Publication Date: 2010-07-28
YUNNAN UNIV
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  • Abstract
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  • Claims
  • Application Information

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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
The selected reaction temperature range for the synthesis of zinc selenide is 270-300°C. Since the reaction temperature is not high enough, the resulting nanocrystals have surface defects and the crystals are not dense.
[0005] In a word, the deficiencies in the current synt

Method used

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  • Method for synthesizing bar-shaped ZnSe fluorescence nanocrystalline
  • Method for synthesizing bar-shaped ZnSe fluorescence nanocrystalline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Synthesis of rod-shaped ZnSe nanocrystals:

[0049] 1. First, heat Se (0.048g, 0.6mmol), TOP (2*0.5g) in an oil bath at 40°C under the protection of nitrogen, and stir for one hour to obtain a Se precursor.

[0050] 2. Combine ODE (2g), ZincStearate (0.054g, 8.5*10 -5 mol), ODA (0.108g) was stirred and mixed under the protection of nitrogen to obtain the Zn precursor. The Zn precursor was "activated" by stirring at 50 °C for 3 hours.

[0051] 3. Octadecyl mercaptan (2.2925g, 8*10 -3 ) was added to the Zn precursor under the protection of nitrogen, and then stirred at 50°C for 1 hour to carry out "template" treatment.

[0052] 4. Continue to raise the temperature of the Zn precursor system to 305°C under the protection of nitrogen, and quickly inject the Se precursor into the Zn precursor while stirring. At this time, the temperature of the reaction system drops to 275°C, and the nanocrystals begin to grow. start the timer.

[0053] 5. After the nanocrystals start t...

Embodiment 2

[0056] 1. First, Se (0.048g, 0.6mmol), TOP (2*0.5g) was heated at 40°C under argon protection and ultrasonicated for half an hour to obtain the Se precursor.

[0057] 2. Combine ODE (2g), ZincStearate (0.0632g, 0.1*10 -3 mol), ODA (0.216g) was stirred and mixed under the protection of argon to obtain the Zn precursor. The Zn precursor was "activated" by ultrasonication at 70°C for 1 hour.

[0058] 3. Octadecyl mercaptan (2.2925g, 8*10 -3 ) was added to the Zn precursor under the protection of nitrogen, and then stirred at 50°C for 1 hour to carry out "template" treatment.

[0059] 4. Continue to raise the temperature of the Zn precursor system to 305°C under the protection of argon, and quickly inject the Se precursor into the Zn 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.

[0060] 5. After the nanocrystals start to grow, when the reaction time reaches 1 hour,...

Embodiment 3

[0063] 1. First, Se (0.048g, 0.6mmol) and TOP (2*0.5g) were heated at 40°C under nitrogen protection and ultrasonicated for half an hour to obtain the Se precursor.

[0064] 2. Combine ODE (2g), ZincStearate (0.054g, 8.5*10 -5 mol), the Zn precursor composed of hexadecylamine (2.16g) was fully ground at room temperature for 3 hours to realize its "activation" treatment.

[0065] 3. Octadecyl mercaptan (1.1462g, 4*10 -3 ) was added to the Zn precursor under the protection of nitrogen, and then stirred at 50°C for 1 hour to carry out "template" treatment.

[0066] 4. Under the protection of nitrogen, raise the temperature of the Zn precursor system to 315°C, and quickly inject the Se precursor into the Zn precursor while stirring. At this time, the temperature of the reaction system drops to 290°C, and the nanocrystals begin to grow, and the reaction start the timer.

[0067] 5. After the nanocrystals start to grow, when the reaction time reaches 1 hour and 30 minutes, stop h...

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Abstract

The invention belongs to a method for synthesizing nanometer materials, in particular to a method for synthesizing bar-shaped ZnSe fluorescence nanocrystalline. The method comprises the following steps: with the protection of inert gas, heating and stirring a simple substance Se or dissolving the simple substance Se in trioctylphosphine phosphine in an ultraphonic manner to obtain Se precursor; dissolving zinc source body in octadecylene and adding activating agent long-chain alkylamine with the protection of inert gas and carrying out activation on the mixture; introducing the long-chain alkyl sulfhydryl to carry out 'template' processing on activated Zn precursor; then with the protection of inert gas, raising temperature to reaction temperature (300-350 DEG C); fast adding Se precursor into the Zn precursor and carrying out reaction for a certain period of time, then obtaining original solution crude product of ZnSe nanocrystalline; adding mixed solvent composed of high-polarity organic solvent and low-polarity organic solvent and washing and centrifuging the mixture; finally using the low-polarity organic solvent to obtain the final product ZnSe nano rod transparent solution. The method has the advantages of simple reaction system, easily available raw materials, small environmental pollution, good degree of crystallization and high fluorescence quantum yield.

Description

technical field [0001] The invention relates to a method for synthesizing nanometer materials. In an organic phase reaction environment, a surfactant is used as a template, and Zn precursor is "templated" to realize the synthesis of rod-shaped ZnSe fluorescent nanocrystals. Background technique [0002] Semiconductor nanomaterials have different physical, chemical and optical properties than bulk materials. Because of its unique photoelectric properties, it has broad application prospects in the fields of biological probes, fuel cells, and nonlinear optics. Studies have shown that the optoelectronic properties of semiconductor nanocrystals are not only related to their composition and size, but also vary with their morphology. For example, one-dimensional nanorods are different from nanopowders. Electronics and optical excitons can only be effectively transported along the axial direction in nanorods, which not only have special properties such as small size effect, surface...

Claims

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Application Information

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IPC IPC(8): C01B19/04B82B3/00C09K11/88
Inventor 蒋峰芝李艳娟
Owner YUNNAN UNIV
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