Method for prehydrolysis preparing core-envelope type inorganic nanocrystalline - silicon dioxide composite grain

A technology of inorganic nano-composite particles, applied in the field of inorganic chemistry, can solve the problems of low yield of core-shell inorganic nano-crystal-silicon dioxide composite particles, adverse effects on the physical and chemical properties of nano-crystals, particle aggregation, etc., and achieve colloidal dispersion The effect of improved ability and chemical stability, simple and easy preparation method, and narrow particle size distribution

Inactive Publication Date: 2008-01-09
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of core-shell inorganic nanocrystalline-silica composite particles prepared by these techniques is low, which is due to the growth of SiO in the ethanol phase. 2 The concentration of core particles added in the cladding layer should not be too high, otherwise particle aggregation will occur
In addition, for metal and semiconductor nanocrystals, ligand exchange reactions are usually required to make the surface of nanocrystals bear silicon-philic groups. Ligand exchange reactions are not only cumbersome to operate, but also usually have adverse effects on the physical and chemical properties of nanocrystals.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1 Fe 3 o 4 Preparation of nanocrystals

[0013] Take 0.5647 g FeCl 3 ·6H 2 O and 0.2077 g FeCl 2 4H 2 O, dissolved in 10ml of deoxygenated high-purity water, added to 60ml of ammonia water with a concentration of 7% under strong stirring, and reacted in a 50°C water bath for 30 minutes. After the reaction is completed, use a 0.1T permanent magnet to separate the black solid from the reaction solution, and wash the obtained solid with deoxygenated high-purity water for 3 to 5 times to obtain Fe with a particle size of 8 to 12 nm. 3 o 4 Nanocrystalline. Fe 3 o 4 nanocrystalline sol. Produced Fe 3 o 4 The concentration of the nanocrystalline sol is about 4mg / ml.

Embodiment 2

[0014] Embodiment 2 Preparation of Au nanocrystals

[0015] 1.2 ml of 80% tetrakishydroxymethylphosphonium chloride (THPC) was dissolved in 100 ml of water. Add 45.5ml of water, 1.5ml of 0.2M NaOH aqueous solution, 1ml of the above THPC solution into a 100ml three-necked flask, and add 4ml of 50mM HAuCl under vigorous stirring 4 The aqueous solution is reacted at room temperature for 30 minutes to obtain a gold nanocrystal sol with a particle diameter of 2-3 nm. The concentration of the prepared Au nanocrystalline sol is about 0.8mg / ml.

Embodiment 3

[0016] Example 3 ZnS: Preparation of Mn nanocrystals

[0017]Add 20ml of water, 25ml 0.1M Zn(Ac)2 into a 100ml three-necked flask, and pass nitrogen gas for 15 minutes, then add 0.870ml mercaptopropionic acid (MPA), 0.75ml 0.1M Mn(Ac)2 and pass nitrogen gas for 3 minutes, use Adjust the pH of 4M NaOH solution to 10.3, and pass nitrogen gas for 15 minutes, and weigh 0.3827g Na2S·9H 2 Dissolve O in 5ml of water, quickly inject it into a three-neck bottle and react for 15 minutes, stop the nitrogen flow, stir in the air for 6 hours, filter it with a filter membrane of φ0.25μm, and put it into the reflux device for reflux for 2 hours (starting with boiling) , after natural cooling, stir and age overnight. Centrifuge at 8000rpm / min for 15 minutes, take the supernatant, heat to boiling, airtightly cool to room temperature. Add ethanol to wash twice, and centrifuge at 8000 rpm / min for 5 minutes to obtain a white precipitate, which is dried in a vacuum desiccator to make a powder. ...

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Abstract

The disclosed method to prehydrolyzed prepare shell-shaped inorganic nano crystal of silicon dioxide composite particle comprises: adding the n-ethyl silicate into the mixed liquid with ammonia, water and ethanol for prehydrolysis; then, adding finished metal oxide, noble metal or semi-conductor nano crystal with known method. This invention needs not any surface finish to obtain the product with regular shape and well chemical property fit to different requests.

Description

technical field [0001] The invention belongs to the field of inorganic chemistry, and in particular relates to a method for coating the surface of nanocrystals to form core-shell composite particles. Background technique [0002] Due to their unique quantum size effects and surface properties, nanocrystals have great application potential in many fields such as photoelectrocatalysis, bioseparation, clinical disease diagnosis, and drug delivery. Using inorganic, organic or polymer materials to coat the surface of nanocrystals to form nanocomposites with a core-shell structure to endow them with good chemical stability and biocompatibility is a necessary solution for the application of nanocrystals in the field of biology. one of the key issues. Among many coating materials, silica is one of the most ideal surface coating materials due to its good chemical stability, optical transparency, colloidal stability, and easy surface modification. [0003] The existing methods for s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/628
Inventor 杨文胜陆子阳戴洁王刚庄家骐
Owner JILIN UNIV
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