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Preparation method of organic-inorganic composite photochromic film material

A photochromic, inorganic composite technology, used in optics, optical components, nonlinear optics, etc., can solve the problems of poor flexibility, high temperature resistance, poor chemical stability, etc., to achieve good wear resistance, high mechanical strength, good The effect of thermal stability

Inactive Publication Date: 2005-06-08
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Past studies on photochromism of heteropoly compounds were limited to in-solution and solid charge-transfer salts, which greatly limited their scope of application
At present, the thin film devices obtained by compounding heteropoly compounds with organic or polymer substrates have insufficient mechanical strength, poor chemical stability, resistance to organic solvents, and high temperature resistance, and because heteropoly acids are easy to form crystals, they are easy to mix with Phase separation of organic or polymeric substrates
However, when the heteropoly compound is combined with the inorganic network (such as the silica network), the rigidity of the inorganic network is too strong, the flexibility is too poor, and the charge transfer efficiency is low due to the influence of the matrix, resulting in poor photochromic response and reversible repeatability. ideal

Method used

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  • Preparation method of organic-inorganic composite photochromic film material
  • Preparation method of organic-inorganic composite photochromic film material

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Dissolve commercial or self-made keggin structure tungstosilicic acid in absolute ethanol to a concentration of 0.5mol L -1 The solution. Dissolve methacrylamide in a mixed solution of toluene and chloroform with a volume ratio of 2:1, and then add vinyltriethoxysilane. Put this mixed solution under the protection of nitrogen, heat the oil bath at a constant temperature of 70°C, then add 0.5% benzoyl peroxide, keep stirring at a high speed, and then add the above-mentioned ethanol solution of tungstosilicate; after the reaction reaches a certain level, add Ethyl orthosilicate, heated in a water bath at 50°C, stirred evenly, then added a mixed solution of water and ethanol drop by drop, keeping H 2 O:Si=4:1, constant temperature for 2 hours. Fix the substrate of quartz glass (or other materials) on the spin coater, drop the colorless and transparent sol on the substrate, control the speed of 1500rpm, rotate for 30 seconds, so that the sol is evenly coated on the substr...

Embodiment 2

[0021] Dissolve commercial or self-made keggin-structure phosphotungstic acid in absolute ethanol to a concentration of 0.5mol L -1 The solution. Dissolve methacrylamide in a mixed solution of toluene and chloroform with a volume ratio of 2:1, and then add vinyltriethoxysilane. Put this mixed solution under the protection of nitrogen, heat it in an oil bath at 70°C, add 0.5% benzoyl peroxide, keep stirring at a high speed, then add the above-mentioned ethanol solution of phosphotungstic acid; Heat in a water bath and stir evenly, then gradually add a mixed solution of water and ethanol dropwise to keep the H 2 O:Si=4:1, stirring at constant temperature for 30 minutes; then adding butyl titanate, in order to prevent the rapid hydrolysis of butyl titanate, add diethanolamine for complexation. Control H at the beginning 2 O:Ti=2:1, gradually reaching 4:1. According to the content of Ti, the obtained sol changes from colorless to orange-red. Fix the substrate of quartz glass ...

Embodiment 3

[0023] Dissolve commercial or self-made keggin structure phosphomolybdic acid in absolute ethanol to a concentration of 0.5mol L -1 The solution. Dissolve methacrylamide in a mixed solution of toluene and chloroform with a volume ratio of 2:1, and then add vinyltriethoxysilane. Put this mixed solution under the protection of nitrogen, heat the oil bath at a constant temperature of 70°C, then add 0.5% benzoyl peroxide, and keep stirring at a high speed, then add the above-mentioned ethanol solution of phosphomolybdic acid; Heat in a water bath at 50°C and stir evenly, then gradually add a mixed solution of water and ethanol dropwise to keep the H 2 O:Si=4:1, stirred at constant temperature for 30 minutes. Then add isopropyl zirconate, in order to prevent rapid hydrolysis of isopropyl zirconate, add ethyl acetoacetate for complexation. Control H at the beginning 2 O:Zr=2:1, gradually reaching 4:1. Fix the substrate of quartz glass (or other materials) on the spin coater, dr...

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Abstract

The invention relates to a preparation method for organic-photic compound millimicron film material with remarkable photo-discoloration performance, its characteristic is that it combines the discoloration molecule self-assembly technology with sol gel course. The following technical steps are included: a. Heteropoly compound keggin structure of tungstosilicic acid, phosphotungstic acid, phosphomolybdic acid are saluted in absolute ethyl alcohol to form solution with a certain density; b. some methyl methacrylate is soluted in the mixture solution of toluene and chloroform then add some vinyltriethoxy silane into it, then it is heated to be 70deg.C in nitrogen and add benzoyl peroxide, stir it greatly until the reaction is complete; c. in the reaction course the heteropoly compound solution is added into; d, the copolymer generated is mixed with metallic alkoxide, benzoyl peroxide in aqueous thermostat and be added with alcohol, abtaining transparent sol solution; e. coat the transparent sol on substrate to be dried for 24 hours, finally the millimicron compound film is acquired.

Description

technical field [0001] The invention relates to a method for preparing an organic-inorganic composite nano film material with good photochromic performance, and belongs to the technical field of special material chemical process manufacturing. Background technique [0002] Heteropoly compounds are a kind of inorganic metal multinuclear complexes containing oxygen bridges, which can be used as electron acceptors to form electron donor-acceptor complexes with organic donors. This type of complexes undergoes electron transfer under light excitation and exhibits photochromic properties. sex. Photochromic materials containing heteropoly compounds have attracted much attention due to their significant application prospects in the fields of information display, sensors, light-adjusting devices and high-density storage. Past studies on the photochromism of heteropoly compounds were limited to solution and solid charge-transfer salts, which greatly limited their application range. ...

Claims

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Application Information

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IPC IPC(8): B05D7/00G02B1/10G02B5/23G02F1/01
Inventor 程知萱黄焱潘庆谊陈海华董哓雯
Owner SHANGHAI UNIV
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