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Zinc sulfide nano particle with sulfydryl surface finish and preparation method thereof

A nanoparticle and surface modification technology, applied in nanotechnology, zinc sulfide, nanotechnology, etc. for materials and surface science, can solve the problems of high activity of hydroxyl and carboxyl groups, lower refractive index, abrupt interface changes, etc., to achieve enhanced Dispersibility, improved bonding, and increased refractive index effects

Inactive Publication Date: 2012-11-07
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect that this method exists is: the content of capping agent in the nanoparticle that is modified by surface modifier is very high, although the refractive index of zinc sulfide nanoparticle itself reaches 2.368, but the refractive index of surface modifier is low (mercaptoethanol n d =1.4996, Thioglycolic acid n d =1.5030), the interface changes abruptly, the refractive index of the modified zinc sulfide nanoparticles will be correspondingly reduced a lot, and the residual hydroxyl and carboxyl groups are highly active, which makes the in-situ polymerization of zinc sulfide nanoparticles and polymer monomers to prepare composite materials. difficult to control

Method used

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  • Zinc sulfide nano particle with sulfydryl surface finish and preparation method thereof
  • Zinc sulfide nano particle with sulfydryl surface finish and preparation method thereof
  • Zinc sulfide nano particle with sulfydryl surface finish and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 0.81g of zinc acetate dihydrate to 50ml of dimethylformamide and mix well, then put it into a three-necked flask and stir it with nitrogen; then add a premix of 1.145g of BES and 25ml of dimethylformamide to the three-necked flask After stirring for 20 minutes, the temperature was raised to 120°C, a premixture of 0.28g thiourea and 25ml dimethylformamide was added, and the mixture was refluxed at 120°C for 10 hours. Then use a vacuum pump to distill and concentrate the reaction product under reduced pressure, precipitate the concentrated solution with ethanol, centrifuge the obtained zinc sulfide particles, wash 3 times with ethanol, wash 2 times with methanol, and dry in vacuum to obtain white powdery zinc sulfide nanoparticles. In this implementation, zinc source / sulfur source / modifier thiol=1 / 1 / 3 (molar ratio).

[0028] Prepare the resulting product by this embodiment, its X-ray diffraction analysis is as follows: figure 1 As shown, the abscissa angle in the fi...

Embodiment 2

[0030] Add 0.81g of zinc acetate dihydrate to 50ml of dimethylformamide, mix well, put it into a three-necked flask and stir with nitrogen; then add a premixture of 1.145g of BES and 25ml of dimethylformamide to the three-necked flask After stirring for 20 minutes, the temperature was raised to 150°C, a premixture of 0.28g thiourea and 25ml dimethylformamide was added, and the mixture was refluxed at 120°C for 10 hours. Then use a vacuum pump to distill and concentrate the reaction product under reduced pressure, precipitate the concentrated solution with ethanol, centrifuge the obtained zinc sulfide particles, wash 3 times with ethanol, wash 2 times with methanol, and dry in vacuum to obtain white powdery zinc sulfide nanoparticles. In this example, zinc source / sulfur source / modifier thiol=1 / 1 / 3 (molar ratio). The zinc sulfide nanoparticles prepared in this example have the same structure as the microspheres prepared in Example 1, and have the same excellent performance.

Embodiment 3

[0032] Add 0.81g of zinc acetate dihydrate to 50ml of dimethylformamide, mix well, put it into a three-necked flask and stir with nitrogen; then add a premixture of 1.145g of BES and 25ml of dimethylformamide to the three-necked flask After stirring for 20 minutes, the temperature was raised to 150°C, a premixture of 0.558g thiourea and 25ml dimethylformamide was added, and the mixture was refluxed at 120°C for 8 hours. Then use a vacuum pump to distill and concentrate the reaction product under reduced pressure, precipitate the concentrated solution with ethanol, centrifuge the obtained zinc sulfide particles, wash 3 times with ethanol, wash 2 times with methanol, and dry in vacuum to obtain white powdery zinc sulfide nanoparticles. In this example, zinc source / sulfur source / modifier thiol=1 / 2 / 3 (molar ratio). The zinc sulfide nanoparticles prepared in this example have the same structure as the microspheres prepared in Example 1, and have the same excellent performance.

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Abstract

Provided are a zinc sulfide nano particle with sulfydryl surface finish and a preparation method thereof. A solvent heat synthesis method is adopted, thiourea is selected to serve as a sulfur source, zinc acetate is a zinc source, and N,N-dimethylformamide serves as a reaction medium. 2,3-dimercaprol ethyl sulfo-propanethiol (BES) serves as dressing agent ligand which is mixed with zinc and the sulfur source according to certain proportion, reaction is carried out for 6-12 hours at the temperature of 120-160 DEG C through condensation backflow, the zinc sulfide nano particle with the sulfydryl surface finish is synthetized in situ, particles are even in dispersion, and average size is within 100nm. The zinc sulfide nano particle provided with the sulfydryl surface finish and obtained by using the preparation method is high in interface refractive index, good in dispersibility and moderate in reaction, contribute to in situ polymerization compound with macromolecules, can serve as an electroluminescence material, is particularly suitable to compound with optic plastic to improve refractive index, and serves as optical elements such as a lens.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a zinc sulfide nanoparticle and a preparation method thereof, in particular to a zinc sulfide nanoparticle with mercapto group surface modification and a preparation method thereof. technical background [0002] Controlled synthesis of zinc sulfide nanoparticles is an important research direction in the field of nanoparticles. The bulk ZnS crystalline material has a high refractive index (n 620nm =2.36), is a semiconductor material with a wide bandgap, and has low light absorption characteristics in a wide range of wavelengths (400-14000nm), and has good optical properties. Therefore, it is often introduced into polymer materials to improve the refractive index and other properties of polymer materials. [0003] At present, the main way to prepare zinc sulfide nanoparticles by chemical method is to adopt water-soluble surfactants (such as mercaptoethanol (CN 102061...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/08B82Y30/00
Inventor 盛维琛谈静吴萍陈桥曹顺生张蓉仙
Owner JIANGSU UNIV
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