Method for preparing selenium-containing compound nano crystal

A technology of selenium compounds and nanocrystals, applied in the direction of selenium/tellurium compounds, binary selenium/tellurium compounds, chemical instruments and methods, etc. Problems such as poor quality and high price, achieve the effect of half-height width and narrow width, cost saving, and uniform size distribution

Inactive Publication Date: 2008-09-17
王小萍
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, Peng et al. and other groups have been using tributylphosphine (TBP) or trioctylphosphine (TOP) to dissolve selenium as the precursor of selenium when synthesizing the precursor of selenium. The disadvantage is that tributylphosphine or trioctylphosphine are toxic, flammable and explosive drugs, and they are expensive
In 2005, Zou Bingsuo's group discovered that dissolving

Method used

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  • Method for preparing selenium-containing compound nano crystal
  • Method for preparing selenium-containing compound nano crystal
  • Method for preparing selenium-containing compound nano crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Take 0.12mmol of cadmium oleate, 0.24mmol of octadecylamine, and 4g of octadecene, mix them into a 25mL three-neck bottle, and heat to 280°C under a nitrogen atmosphere until the solution is completely uniform; mix 1.2mmol of Se powder, 3.6mmol of octadecylamine and 10ml Octadecene is mixed and heated at 220°C to obtain a light yellow selenium precursor solution. Take 2mL of selenium precursor solution and quickly inject it into a three-necked bottle, and then lower the temperature to 260°C for growth. The solution is colorless when it is first injected, and then gradually turns into light yellow, yellow, light red, red, deep red, dark red, and the reaction time is three hours. When the solution is of different colors, CdSe nanocrystals of different sizes can be obtained. . The solutions of different colors were sampled for fluorescence spectrum and absorption spectrum test, and the fluorescence peak changed from 470nm to 650nm. Fluorescence spectrum such as figure 1 ...

Embodiment 2

[0023] Take 0.12mmol of cadmium oxide, 0.3mmol of oleic acid, and 3.8g of octadecene and mix them into a 25mL three-neck bottle, and heat to 260°C under a nitrogen atmosphere until the solution is completely uniform; mix 1.2mmol of Se powder, 3.6mmol of octadecylamine and 10ml of Decene was mixed and heated at 220°C to obtain a light yellow selenium precursor solution. Take 3mL of selenium precursor solution and inject it into the three-necked bottle quickly, and then lower the temperature to 240°C for growth. The solution is colorless when it is just injected, and then gradually turns into light yellow, yellow, light red, red, deep red, dark red, and the reaction time is two hours. When the solution is of different colors, CdSe nanocrystals of different sizes can be obtained. . The solutions of different colors were sampled for fluorescence spectrum and absorption test, and the fluorescence peak changed from 470nm to 620nm.

Embodiment 3

[0025] Take 0.12mmol of cadmium stearate, 1.2mmol of octadecylamine, and 5g of tetradecane and mix them into a 25mL three-neck bottle, and heat to 240°C under nitrogen until the solution is completely uniform; mix 1.2mmol of Se powder, 3.6mmol of oleic acid and Mix 10ml of liquid paraffin and heat at 220°C to obtain a light yellow selenium precursor solution. Take 4mL of selenium precursor solution and quickly inject it into a three-necked bottle, then lower the temperature to 260°C for growth. The solution is colorless when it is first injected, and then gradually turns into light yellow, yellow, light red, red, deep red, dark red, and the reaction time is three hours. When the solution is of different colors, CdSe nanocrystals of different sizes can be obtained. . The solutions of different colors were sampled for fluorescence spectrum and absorption test, and the fluorescence peak changed from 470nm to 650nm.

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Abstract

The invention relates to a preparation method of selenium-bearing compound nanocrystal, which comprises following steps: heating the precursor of the twelve family elements to 240 to 380 DEG C in inertia environment; mixing with the selenium precursor at 20 to 300 DEG C; enabling the growth of the mixture at 240 to 380 DEG C for 1 to 12 hours to obtain the selenium-bearing compound nanocrystal; wherein, the selenium precursor is obtained by dissolving selenium salt in the solvent with additives; the additives are organic amine or organic acid with the carbon content of no less than 10; the solvent is non-coordinating solvent with the dissolving point of no more than 60 DEG C; the molar ratio of the additives and the selenium is 3 to 5:1. The method has the advantages of regular and stable low toxicity medicine for synthesis, economy, environmental friendliness, capability of saving cost of over 80%, high quality of nanocrystal, even size distribution, high fluorescence efficiency, narrow FWHM (full width at half maximum), and huge application value in both laboratory synthesis and industrial synthesis.

Description

(1) Technical field [0001] The invention relates to a preparation method of a selenium-containing compound nanocrystal, in particular to a method for synthesizing a high-quality selenium-containing compound nanocrystal without phosphorus. (2) Background technology [0002] Semiconductor nanoparticles, especially II-VI semiconductor nanoparticles are research hotspots in recent years. Semiconductor nanoparticles are also called semiconductor quantum dots (Quantum Dots, referred to as QDs). Due to their relatively small size, ranging from a few to a dozen nanometers, they will produce many physical and chemical properties that bulk materials do not have, such as quantum size effect, dielectric confinement effect, surface effect, etc., which make it have broad application prospects in optoelectronic devices, solar cells, and laser biomarkers. Recently, research on semiconductor nanocrystals in the visible light-emitting region, especially as a biomarker, has attracted attentio...

Claims

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Application Information

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IPC IPC(8): C01B19/00C01B19/04
Inventor 李林松申怀彬
Owner 王小萍
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