Low-cost method for synthesizing ZnxCd1-xSe (x is more than or equal to zero and less than or equal to 1) and related core/shell structured semiconductor nanocrystals thereof

A synthesis method and nanocrystal technology, applied in chemical instruments and methods, selenium/tellurium compounds, inorganic chemistry, etc., can solve the problems of complex nanocrystal process, high synthesis cost, harsh reaction conditions, etc. The effect of preparation cost and simple process

Inactive Publication Date: 2010-11-24
HENAN UNIVERSITY
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Problems solved by technology

[0003] The object of the present invention is to provide a simple and efficient, low-cost, no phosphine compound participation, good repeatability and large-scale synthesis of high-quality Zn x Cd 1-x Se(0≤x≤1), Zn x Cd 1-x Se / ZnSe, Zn x Cd 1-x Se / ZnS and Zn x Cd 1-x Se / ZnSe / ZnS semiconductor nanocrystal method to solve the current problems of complex preparation process of nanocrystals, harsh reaction conditions and high synthesis cost

Method used

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  • Low-cost method for synthesizing ZnxCd1-xSe (x is more than or equal to zero and less than or equal to 1) and related core/shell structured semiconductor nanocrystals thereof
  • Low-cost method for synthesizing ZnxCd1-xSe (x is more than or equal to zero and less than or equal to 1) and related core/shell structured semiconductor nanocrystals thereof
  • Low-cost method for synthesizing ZnxCd1-xSe (x is more than or equal to zero and less than or equal to 1) and related core/shell structured semiconductor nanocrystals thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Synthesis of ZnSe (x=1) nanocrystals: Take 2mL of Se precursor solution (2mmol (0.16g) Se and 20mL of octadecene mixed into a 50mL three-neck flask, and heat at 220°C for 3 hours to obtain a light yellow Se precursor solution) and 4mL of octadecene were mixed into a 25mL three-neck bottle, and when heated to 260°C under nitrogen protection, 1mL of zinc precursor solution (2mmol (1.254g) zinc oleate dissolved in 10mL of liquid paraffin) was quickly injected into growing in the above solution and cooling down to 240° C. to obtain ZnSe nanocrystals. Take samples at 10s, 5min, and 1h to obtain the fluorescence spectrum as figure 1 (x=1), the fluorescence range is 400-450nm, the half-peak width is between 14-17nm, the quantum yield is 40-60%, and the absorption spectrum is as figure 2 (x=1), the final synthesized ZnSe nanocrystal XRD and TEM pictures are as image 3 (x=1).

Embodiment 2

[0024] Synthetic Zn 0.995 Cd 0.005 Se (x = 0.995) nanocrystals: Take 2mL Se precursor solution (2mmol (0.16g) Se and 20mL octadecene are mixed and added to a 50mL three-neck flask, and heated at 220°C for 3 hours to obtain a light yellow Se precursor solution ) and 4mL of octadecene were mixed into a 25mL three-neck flask, and when heated to 280°C under nitrogen protection, 1mL of zinc and cadmium precursor solutions (1.99mmol (1.248g) zinc oleate and 0.01mmol (respectively) (0.00674g) cadmium oleate was dissolved in 10mL liquid paraffin to obtain zinc and cadmium precursors) was injected into the above solution, and cooled to 260°C to grow to obtain Zn 0.995 Cd 0.05 Se nanocrystals. Take samples at 10s, 1min, 5min, 30min, and 1h (from bottom to top) to obtain the fluorescence spectrum as figure 1 (x=0.995), the fluorescence peak position is 456nm, the quantum yield is 55%, and the half-maximum width is 33nm, and the absorption spectrum is as follows figure 2 (x=0.995). ...

Embodiment 3

[0026] Synthetic Zn 0.99 Cd 0.01 Se (x=0.99) nanocrystals: Take 2mL of Se precursor solution (2mmol (0.16g) Se and 20mL of octadecene are mixed and added to a 50mL three-neck flask, and heated at 220°C for 3 hours to obtain a light yellow Se precursor solution ) and 4mL of octadecene were mixed into a 25mL three-neck bottle, and when heated to 300°C under nitrogen protection, 1mL of the precursor solution of zinc and cadmium (1.98mmol (1.251g) zinc stearate and 0.02mmol (0.01356 g) cadmium stearate (dissolved in 10mL liquid paraffin) is injected into the above solution, and cooled to 280 ° C to grow, that is, to obtain Zn 0.99 Cd 0.01 Se nanocrystals. Take samples at 10s, 1min, 5min, 30min, and 1h to obtain the fluorescence spectrum as figure 1 (x=0.99, from bottom to top), the fluorescence peak position is 467nm, and the quantum yield is 60%, and the width at half maximum is 35nm, and absorption spectrum is as figure 2 (x=0.99), the Zn that finally gets 0.99 Cd 0.01 S...

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Abstract

The invention provides a method for synthesizing ZnxCd1-xSe (x is more than or equal to 0 and less than or equal to 1) and ZnxCd1-xSe/ZnSe, ZnxCd1-xSe/ZnS and ZnxCd1-xSe core/shell structured semiconductor nanocrystals thereof by using long-chain fatty acid salts of cadmium and zinc as precursors of cadmium and zinc, which is the most economical and environment-friendly method for synthesizing high-quality ZnxCd1-xSe and related core/shell structured semiconductor nanocrystals thereof currently. The method avoids using tributylphosphine (TBP) or trioctylphosphine (TOP) dissolved elementary selenium as the precursor of selenium currently in the world, but adopts octadecylene (ODE) dissolved elementary selenium as the precursor of selenium; and the obtained nanocrystals have the quality equal to that of nanocrystals which are synthesized when the TBP or TOP dissolved selenium powder is used as the precursor of selenium. The method is called a phosphine-free method, has the advantages of simple synthesizing process, good repeatability, safety, environmental protection, no need of glove box, and cost conservation of over 60 percent. The synthesized ZnxCd1-xSe and related core/shell structured nanocrystals have a fluorescence range of between 400 and 650nm, and have the advantages of uniform particle size distribution, high efficiency of fluorescent quantum yield (40 to 70 percent) and narrow full width at half maximum. The method is also suitable for synthesizing the ZnxCd1-xS, HgxCd1-xSe, ZnxCd1-xTe nanocrystals and related core/shell structures thereof. More importantly, the method can synthesize high-quality nanocrsytals on a large scale, and has enormous application value both in laboratory synthesis and industrial synthesis.

Description

technical field [0001] The invention relates to a low-cost, environment-friendly, simple and controllable method for synthesizing high-quality semiconductor nanocrystals. The method can be produced on a large scale, so it has great application value in the industrial synthesis of fluorescent nanocrystal materials. Background technique [0002] Fluorescent nanocrystals, especially Ⅱ-Ⅵ semiconductor nanoparticles are research hotspots in recent years. Fluorescence with different wavelengths can be generated by adjusting the size of nanocrystals, and has attracted much attention due to its potential applications in biomolecular labeling and immunodetection, light-emitting diodes, lasers, and solar cells. In previous literature reports, CdSe, ZnSe, Zn x Cd 1-x Most of the selenium precursors used in the process of nanocrystallization such as Se are obtained by dissolving simple selenium in phosphine-containing compounds such as tributylphosphine (TBP) or trioctylphosphine (TO...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/00C09K11/88
Inventor 李林松申怀彬
Owner HENAN UNIVERSITY
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