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Method for synthesizing super small-size CdSe nanocrystalline through one-pot process

A small-sized, nanocrystalline technology, applied in the fields of nanotechnology, nano-optics, nanotechnology, etc., can solve the problems of poor stability of ultra-small-sized nanocrystals, environmentally harmful phosphine compounds, single ultra-small nanocrystals, etc., and achieve nucleation. Stable and controllable growth rate, good operability and repeatability, and low synthesis cost

Inactive Publication Date: 2014-02-05
GUANGXI UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

In short, the shortcomings of the thermal injection method for preparing ultra-small nanocrystals are: (1) most of the organic phosphines are used as ligands or solvents, and the phosphines are not only harmful to the environment, but also expensive; (2) the prepared ultra-small nanocrystals Poor stability, it can only be stable for a short period of time during the reaction process, and as the reaction progresses, it quickly evolves into larger or conventional size nanocrystals; (3) it is not easy to obtain ultra-small nanocrystals with a single size, often coexisting in various sizes, Ultra-small nanocrystals of a single size must be obtained through complex size screening methods; (4) The high-temperature thermal injection method itself is not easy to control and has poor repeatability, which is not conducive to batch preparation

Method used

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  • Method for synthesizing super small-size CdSe nanocrystalline through one-pot process
  • Method for synthesizing super small-size CdSe nanocrystalline through one-pot process
  • Method for synthesizing super small-size CdSe nanocrystalline through one-pot process

Examples

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Effect test

Embodiment 1

[0028] Example 1: Preparation of ultra-small size CdSe nanocrystalline F461 species

[0029] Mix 0.022g (0.2mmol) selenium dioxide and 2mL N-oleoyl morpholine, raise the temperature under magnetic stirring until the selenium dioxide is completely dissolved, and then cool to room temperature to obtain the Se precursor;

[0030] Mix 0.213g (0.8mmol) cadmium acetate dihydrate and 3mL N-oleoyl morpholine, stir and heat until the cadmium acetate dihydrate is completely dissolved, then cool to room temperature to obtain the Cd precursor;

[0031] Mix the above two solutions, heat under stirring, start timing at a heating rate of 15°C / min to 210°C, and take samples at different growth times, inject the taken samples into cold toluene, add methanol to precipitate out For the crude product of nanocrystals, the volume ratio of the added precipitant to the nanocrystal solution is 2:1, the crude product is then dissolved in toluene, the precipitant is precipitated, and centrifuged, and tr...

Embodiment 2

[0036] Embodiment 2: Preparation of ultra-small size CdSe nanocrystals emitting white light

[0037] Mix 0.022g (0.2mmol) of selenium dioxide and 2mL of N-oleoyl morpholine, raise the temperature under magnetic stirring until the selenium dioxide is completely dissolved, and then cool to room temperature to obtain the Se precursor;

[0038] Mix 0.213g (0.8mmol) cadmium acetate dihydrate, 0.200g (1mmol) lauric acid and 3mL N-oleoyl morpholine, stir and heat until the cadmium acetate dihydrate is completely dissolved, then cool to room temperature to obtain the Cd-lauric acid precursor ;

[0039] Mix the above two solutions, heat under stirring, start timing at a heating rate of 10°C / min to 150°C, and take samples at different growth times, inject the taken samples into cold toluene, add methanol to precipitate out For the crude product of nanocrystals, the volume ratio of the added precipitant to the nanocrystal solution is 2:1, the crude product is then dissolved in toluene, ...

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Abstract

The invention discloses a method for synthesizing super small-size CdSe nanocrystalline through a one-pot process, relating to the technical field of a preparation method of semiconductor nanocrystalline. The method comprises the following synthesis steps of respectively preparing a Se precursor solution and a Cd precursor solution; mixing the two precursor solutions, stirring, heating, and rapidly raising the temperature to be 150-240 DEG C at a speed of 10 to 20 DEG C per minute; synthesizing for 10-300 minutes at a growth temperature, thereby preparing the super small-size CdSe nanocrystalline. Compared with the prior art, the method has the advantages that the synthesized super small-size CdSe nanocrystalline is simple in synthesis operation and environment-friendly and has high repeatability, the synthesis cost is low, and the obtained super small-size CdSe nanocrystalline is single in size, high in quality and stable in performance.

Description

technical field [0001] The invention relates to the technical field of semiconductor nanocrystal preparation methods, in particular to a method for synthesizing ultra-small CdSe nanocrystals in one pot. Background technique [0002] Ultra-small-sized semiconductor nanocrystals (magic-sized semiconductor nanocluster in English) are defined as molecular clusters with a highly symmetrical closed-shell structure and a size of 1-2 nm. Unlike conventional size (>2nm) nanocrystals that have a strong quantum size effect, ultra-small semiconductor nanocrystals have a fixed size, a sharp absorption peak with a constant wavelength, and a size accurate to the atomic scale. Another important feature is that their specific surface area is particularly high, with more than 90% of the atoms occupying the surface of the particles, while only about 22% of the atoms occupy the surface of the nanocrystals with a particle size of 4 nm. Therefore, ultra-small semiconductor nanocrystals have s...

Claims

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Application Information

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IPC IPC(8): C01B19/04C09K11/88B82Y40/00B82Y20/00
Inventor 刘新梅傅凤鸣黄文艺黄琼
Owner GUANGXI UNIVERSITY OF TECHNOLOGY
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