Preparation method of nano particles with high refractive index and polymer nano composite film material

A nanoparticle and high refractive index technology is applied in the field of preparing nanocomposite thin film materials after high refractive index nanoparticles are compounded with polymers, which can solve the problems of poor film formation, poor water resistance of composite materials, and poor material stability, etc. Achieve the effect of uniform optical properties, simple process and good stability

Inactive Publication Date: 2003-02-05
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the water-soluble polymer, the final composite has poor water resistance and poor mechanical strength
In addition, inorganic nanoparticles exist in the polymer in the form of simple doping, and there is no chemical bond between the particles and polymer molecules, so the nanoparticles are easy to aggregate in the polymer matrix, and the stability of the material is poor
Although TiO 2 / Polymer hybrid materials can overcome the above disadvantages, but such materials have a large shrinkage rate during the curing process and poor film-forming properties, which will eventually affect the optical and mechanical properties of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: the synthesis (1) of the ZnS colloidal nanoparticle of surface modification

[0020] On an ice bath, under vigorous stirring, in 100ml of 0.5M anhydrous zinc acetate / dimethylformamide (DMF) solution containing 0.2M thiophenol and 0.1M mercaptomethylstyrene, an excess of 6-fold Dry hydrogen sulfide gas equivalent to zinc acetate, control the feed rate to 0.5 ml / min, and finally remove excess hydrogen sulfide gas with nitrogen to obtain a colorless and transparent ZnS nano-sol.

[0021] Observation of surface-modified ZnS nanoparticles by transmission electron microscope (TEM) shows that the particle size is 2-5 nanometers, and electron diffraction and X-ray diffraction show that ZnS particles have a cubic structure. The ZnS nanometer sol obtained above is vacuum-dried to obtain surface-modified ZnS nanoparticle powder through infrared characterization results as follows (KBr): ν (cm -1 ): 3404, 2920, 2855, 1647, 1629, 1603, 1577, 1508, 1406~1477cm -1 , 69...

Embodiment 2

[0022] Embodiment 2: the synthesis (2) of the ZnS colloidal nanoparticle of surface modification

[0023] Except replacing mercaptomethylstyrene with mercaptoethanol, other conditions are the same as in Example 1.

[0024] Analysis shows that the particle size of ZnS particles is also 2-5 nanometers, and the crystal form is cubic structure. The chemical composition of the surface-modified ZnS nanoparticles is Zn 2+ :S 2- : RS - =1:0.78:0.6.

[0025] Similarly, in the above embodiments, the surface modifier can be pure thiophenol, mercaptomethylstyrene or mercaptoethanol, etc., and their respective concentrations can vary between 0.1-0.5M.

[0026] The same method as above can be used to prepare nano-ZnS colloids with other types of surface modifiers.

Embodiment 3

[0027] Embodiment 3: Synthesis and polymerization of polyurethane acrylate macromonomer

[0028] Dissolve 15.4g of 2,2'-dimercaptoethylsulfide (MES) and 26.1g of 2,4'-toluene diisocyanate (TDI) in 100ml of anhydrous dimethylformamide (DMF) solution, add a small amount dibutyltin dilaurate as catalyst. The reaction mixture was reacted at 55° C. for 4 hours under the protection of nitrogen, then 6.5 g of hydroxyethyl methacrylate was added dropwise, and the reaction was continued for 2 hours to finally obtain a DMF solution of 23 wt % polyurethane acrylate macromonomer. IR Spectrum (KBr): ν(cm -1) 3292, 3047, 2930, 2924, 2857, 1726, 1654, 1639, 1618, 1602, 1540, 1454, 1448, 1418, 1300, 1215, 1194, 1031, 878, 815, 768. IR spectrum analysis results show that 1639cm -1 The peak is the characteristic peak of methacrylate double bond, 1654, 3239cm -1 It is the characteristic vibration peak of polyurethane bond, while the characteristic peaks of mercapto group and isocyanate disap...

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Abstract

The preparation method of nano composite film material by using nano microparticles with high refractive index and polymer includes the following three steps: preparing ZnS nano microparticles for surface modification, preparing organic polymer monomer and polymer with high refractive index and preparing nano composite film. In the organic solvent of zinc metal salt the organic small molecule surface modifier with function group is added, and the hydrogen sulfide gas is introduced to synthesize ZnS nano colloidal microparticles, and the polymer base material for combining ZnS nano microparticles can be polymethyl methacrylate, polybutyl methacrylate, polystyrene, epoxyresin, polymer large monomer, optimally can be polyurethane oligomer and polyurethane acrylate large monomer with high refractive index, finally the above-mentioned materials can be made into the invented nano composite film.

Description

Technical field: [0001] The invention relates to a method for preparing a high-refractive-index film material, in particular to a method for preparing a nano-composite film material after compounding high-refractive-index nano particles and polymers. The thin film material synthesized by this method can be used to construct surface anti-reflection coatings of optical devices, display devices and solar cells. technical background: [0002] Currently, high refractive index optical coatings are mainly divided into two categories: polymer optical coatings and inorganic optical coatings. Polymer optical coatings have the advantages of light weight, impact resistance, and easy processing and molding. However, the polymer surface has low hardness, poor heat resistance, and a narrow range of refractive index (n d between 1.35 and 1.7). Although some special polymers such as polythiophene have a higher refractive index (n=2.12), they have strong optical absorption coupling in the v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08K3/30C08L25/06C08L33/10C08L63/00C08L75/04
Inventor 吕长利崔占臣杨柏
Owner JILIN UNIV
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