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Method for preparing inorganic nanoparticle/aromatic polyimide composite film and composite film prepared according to method

A polyimide film, inorganic nanoparticle technology, applied in the direction of coating, can solve the problems of low interface bonding strength, low selectivity, molecular weight drop, etc. The effect of improving selectivity

Active Publication Date: 2018-10-09
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high chemical reactivity of the fluorine gas in the fluorine / nitrogen gas mixture used, the selectivity of its chemical reaction with the macromolecular chains on the surface of the polyimide film is not strong, and it will react with the polyimide macromolecules. Chemical reactions at multiple sites on the chain, including main chain scission reactions
Although this main chain scission behavior may produce more active sites, it will obviously lead to the scission of the macromolecular chains on the surface of the polyimide film, and the molecular weight will be significantly reduced (forming small molecules), which will make the interfacial bonding strength of the subsequent formation not actually high
At the same time, simply increasing the fluorination intensity will only lead to the occurrence of more macromolecular chain scission behaviors, that is, it is impossible to greatly increase the number of subsequent derivatizable grafting reactive groups.

Method used

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  • Method for preparing inorganic nanoparticle/aromatic polyimide composite film and composite film prepared according to method
  • Method for preparing inorganic nanoparticle/aromatic polyimide composite film and composite film prepared according to method
  • Method for preparing inorganic nanoparticle/aromatic polyimide composite film and composite film prepared according to method

Examples

Experimental program
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Effect test

Embodiment 1

[0059] First prepare the polyimide film with the monomer molar ratio of BPDA:PABZ=1:1, and then statically soak the film in Fe 3+ The mass concentration is 0.02g / mL, and the volume concentration of water is 1% ethanol solution, after the complexation reaction 6h, dry, and then pass through the concentration of 200Pa / g F 2 / N 2 (F 2 The volume fraction is 10%) fluorination for 20min, followed by static immersion at 80°C in an ethanol solution containing 50% aminopropyltriethoxysilane by mass fraction of the solution, reacting for 3h and drying, then statically immersing the membrane in pH =3 in nitric acid aqueous solution for 10 minutes and then dried, and finally hydrolyzed tetraethyl orthosilicate with a hydrochloric acid catalytic concentration of 50% of the mole fraction of the solution to obtain silica sol, which was spin-coated twice on the film and baked at 100°C Just dry for 10 hours.

Embodiment 2

[0061] First prepare a polyimide film with a monomer molar ratio of BPDA:PMDA:ODA:PABZ=1:1:1:1, and then statically soak the film in Ni 2+ The mass concentration is 0.01g / mL, and the volume concentration of water is 1% ethanol solution, after the complexation reaction for 1h, it is dried, and then the F with a concentration of 1000Pa / g is passed through 2 / N 2 (F 2 The volume fraction is 10%) fluorination for 1min, followed by static immersion at 30°C in an ethanol solution containing 10% of the solution mass fraction of aminopropyltrimethoxysilane and 10% of the solution mass fraction of 3-aminopropyltrihydroxysilane In the process, dry after reacting for 5 hours, then statically immerse the film in an aqueous solution of oxalic acid with pH=6 for 60 minutes and then dry it for 60 minutes, and finally hydrolyze aluminum isopropoxide with a phosphoric acid catalytic concentration of 90% of the mole fraction of the solution to obtain an aluminum sol. Immerse the film in the s...

Embodiment 3

[0063] First prepare the polyimide film with the monomer molar ratio of BPDA:PDA:PABZ=10:9:1, and then statically soak the film in Cu 2+ The mass concentration is 0.015g / mL, the volume concentration of water is in the ethanol solution of 0.5%, dry after 8h of complexation reaction, then feed the F with concentration of 500Pa / g 2 / N 2 (F 2 10% by volume) fluorination for 5 minutes, then statically soaked in an ethanol solution containing 3-mercaptopropyltriethoxysilane with a mass fraction of 50% of the solution at 90°C, reacted for 1 hour, dried, and then statically soaked the membrane After hydrolysis reaction in aqueous sulfuric acid solution with pH=3 for 30 minutes, dry it, and finally hydrolyze butyl titanate with nitric acid catalytic concentration of 1% of the mole fraction of the solution to obtain titanium sol, immerse the film in the sol and pull it 5 times, and bake at 40°C Just dry for 24 hours.

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Abstract

The invention relates to a method for preparing an inorganic nanoparticle / aromatic polyimide composite film and the composite film prepared according to the method. The method comprises the followingsteps: complexing an aromatic polyimide film containing an imidazole structure and heavy metal ions; fluorating the aromatic polyimide film of which the surface is complexed with the heavy metal ionsto obtain a polyimide film of which the surface contains fluorocarbon bonds; introducing silicon hydroxyl to the polyimide film through the fluorocarbon bonds to form a polyimide film of which the surface contains silicon hydroxyl; introducing an inorganic nanoparticle layer through the silicon hydroxyl to obtain the composite film. With the adoption of the method, the selectivity of the fluorating reaction can be improved, so that the content of C-F bond on the surface of the polyimide film is increased, and chain scission of polyimide macromolecules can be avoided; the composite film is highin stem grafting density, elemental oxygen resistance and corona resistance.

Description

technical field [0001] The invention relates to the field of aromatic polyimide films, in particular to a method for preparing an inorganic nanoparticle / aromatic polyimide composite film and the prepared composite film. Background technique [0002] Aromatic polyimide (polyimide) is a high-performance polymer material with good mechanical properties, thermal properties and chemical stability. It plays an important role in aerospace, energy, electronics, etc. It is often used in Used as solar cell substrates, liquid crystal displays, gas separation membranes, etc. When used in some specific situations such as low-earth orbit, high-speed rail motors, and high-voltage power transmission and transformation, polyimide materials are required to have properties such as atomic oxygen resistance and corona resistance. The more economical and convenient method is to coat the surface of polyimide film Apply a protective inorganic coating with excellent resistance to atomic oxygen and ...

Claims

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Application Information

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IPC IPC(8): C08J7/06
CPCC08J7/06C08J2379/08
Inventor 刘向阳蒋婵程政罗龙波王旭刘昌莉
Owner SICHUAN UNIV
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