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Colorless and transparent polyimide nano-composite material membrane and preparation method thereof

A technology of nanocomposite materials and composite material films, which is applied in the field of polymer-based nanocomposite materials, and can solve the problems of reduced transparency and the like

Inactive Publication Date: 2010-09-15
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These polyimide nanohybrid films exhibit good optical clarity and are nearly colorless, but the transparency decreases slightly with increasing clay content

Method used

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  • Colorless and transparent polyimide nano-composite material membrane and preparation method thereof
  • Colorless and transparent polyimide nano-composite material membrane and preparation method thereof
  • Colorless and transparent polyimide nano-composite material membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Quaternary ammonium salt (CTAB) was used as an intercalant to perform ion exchange modification treatment on montmorillonite to prepare organic montmorillonite. 0.0427 g of organic montmorillonite was added to 6.38 ml of N,N-dimethylacetamide (DMAc) solvent, and dispersed at 80° C. under strong mechanical stirring for 5 hours to obtain a DMAc solution of organic montmorillonite. In a three-necked reaction flask equipped with a stirrer, a thermometer and a nitrogen inlet, 6.5445 g of 2,2-bis[4-(4-amino-2-trifluoromethylphenoxy)phenyl]hexafluoropropane (0.01mol) dissolved in 45ml DMAc solvent, stirred to make the solution clear and transparent. Then add 1.9611g (0.01mol) of 1,2,3,4-cyclobutanetetracarboxylic dianhydride (CBDA) to the solution at one time, stir to dissolve it completely, and continue to react for 15-25 under a nitrogen atmosphere. Within hours, a transparent viscous liquid-polyamic acid (PAA) solution was obtained. The DMAc solution of the above-mentioned...

Embodiment 2

[0046] Will 0.0645g warp? -Aminopropyltriethoxysilane treated nano zinc oxide (particle size 30nm) was dispersed in 27.23ml of DMAc solvent under ultrasonic action, a uniform mixed solution was obtained after 2 hours, and moved to equipped with a stirrer and thermometer And nitrogen gas into the three-necked reaction flask. Dissolve 4.2833 g (0.01 mol) of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene in the above solution, and stir to make the solution clear and transparent. Then add 2.1014g (0.01mol) of 1,2,4,5-cyclopentanetetracarboxylic dianhydride (CPDA) to the solution at once, stir to dissolve it completely, and continue to react for 15-25 under a nitrogen atmosphere. After hours, a transparent viscous liquid-polyamic acid solution with a solid content of 20 wt% by weight is obtained, and the intrinsic viscosity is 1.15 dL / g. Coat the polyamic acid solution on a clean glass plate, place it in a dry box with nitrogen protection, and increase the temperature according ...

Embodiment 3

[0049] In a three-necked reaction flask equipped with a stirrer, a thermometer and a nitrogen inlet, 6.5445 g of 2,2-bis[4-(4-amino-2-trifluoromethylphenoxy)phenyl]hexafluoropropane (0.01mol) was dissolved in 53.08ml of DMAc solvent and stirred to make the solution clear and transparent. Then add 2.2417g (0.01mol) of 1,2,4,5-cyclohexanetetracarboxylic dianhydride (CHDA) to the solution at once, stir to dissolve it completely, and continue to react for 15-25 under a nitrogen atmosphere. After hours, a transparent viscous liquid-polyamic acid solution with a solid content of 15 wt% by weight is obtained, and the intrinsic viscosity is 1.00 dL / g. Add 0.1529 g of tetraethyl orthosilicate (TEOS) and a little water to the polyamic acid solution. After stirring for 20 hours, the mixed solution is coated on a clean glass plate and placed in a dry box protected by nitrogen. The temperature is increased according to the following program: 80°C for 2hrs, 120°C for 1hr, 150°C for 1hr, 200...

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Abstract

The invention relates to a colorless and transparent polyimide nano-composite material membrane and a preparation method thereof. The polyimide nano-composite material membrane is prepared by a method of compounding alicyclic dianhydride and fluorinated diamine serving as monomers with a certain amount of inorganic nano-particles by using nano-composite technology and performing thermal imidization with gradient temperature increase. The amount of added nano-particles is controlled between 0.01 and 5.00 weight percent to obtain the colorless and transparent polyimide nano-composite material membrane with high heat resistance. The membrane has a glass transition temperature of over 250 DEG C, a light transmittance of over 90 percent at 450 nanometers and an ultraviolet wavelength of about 300 nanometers, and can be used as a substrate material for a photoelectric device, a semiconductor material, an optical waveguide material and the like.

Description

Technical field [0001] The invention belongs to the field of polymer-based nano composite materials, and particularly relates to a colorless and transparent polyimide nano composite film and a preparation method thereof. Background technique [0002] Polyimides (PI) is a class of high heat-resistant polymer materials with excellent comprehensive properties, but the general PI is a yellow-brown transparent material, which is mainly due to the intramolecular and molecular It is caused by the easy formation of charge transfer complex (CTC). At present, the following methods are usually used to improve the transparency of PI films: (1) Introduce fluorine-containing substituents or side groups into the PI molecular structure, and use the greater electronegativity of fluorine atoms to cut off the conjugation of the electron cloud and inhibit CTC Formation; (2) Reduce the content of aromatic structure in the PI molecular structure, such as the use of dianhydride or diamine monomers wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/08C08K9/00C08K9/06C08K9/04C08K9/02C08K3/34C08K3/22C08K3/36C08K3/28C08K3/24C08K7/00C08K3/04C08G73/10C08J5/18
Inventor 鲁云华胡知之王永飞房庆旭雷芃张志强肖国勇迟海军董岩赵洪斌李晓王翠苹
Owner UNIV OF SCI & TECH LIAONING
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