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Modified polyimide film

A polyimide film and modification technology, which is applied in the field of polyimide films modified by organically treated carbon black, can solve the problems of poor film formation, poor mechanical properties and large shrinkage rate.

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

AI Technical Summary

Problems solved by technology

In addition, it has a large shrinkage rate during the curing process, and poor film-forming and mechanical properties.

Method used

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Experimental program
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preparation example Construction

[0024] (2) Preparation of the prepolymer of polyimide:

[0025] Put "dianhydride" monomer, "diamine" monomer and organic solvent in a reactor with stirring device, the molar ratio of "dianhydride" monomer to "diamine" monomer is 1: (1.0~ 1.2), under the condition of 10°C to 30°C, stir for 2 hours to 8 hours to obtain the prepolymer of polyimide;

[0026] (3) Preparation of modified polyimide film:

[0027] The carbon black prepared by step (1) and the prepolymer of polyimide prepared by step (2) are placed in a reactor with a stirring device, stirred and mixed to obtain a mixture, and the content of carbon black in the obtained mixture 0.1wt% to 10wt%, use a threaded coating rod or a spin coater to coat the resulting mixture on a film substrate at a spin coating speed of 500 rpm to 3,500 rpm, and use a gradient temperature rise method under vacuum conditions: That is, keep at 60°C to 110°C for 0.5 hours to 5 hours, at 110°C to 250°C for 0.5 hours to 5 hours, and at 250°C to ...

Embodiment 1

[0036] Chemical modification of carbon black surface

[0037] Carbon black (Mougl-L, produced by Cabot Company) was first heated to reflux (oxidize) with a strong acid solution (98% concentrated sulfuric acid and 69% concentrated nitric acid mixed in a volume ratio of 3:1) for more than 4 hours. Then it was washed with distilled water until neutral, vacuum filtered, and dried to obtain acidified carbon black. Add an appropriate amount of thionyl chloride and dimethylformamide to the acidified carbon black, stir it electromagnetically at 70°C for 24 hours, wash it with tetrahydrofuran, separate it by centrifugation, and dry it in vacuum at room temperature to obtain acid chloride-treated carbon black.

[0038] Utilize the laser particle size analyzer to record the average particle diameter of acid chloride carbon black to be 123nm; To acid chloride carbon black is characterized by infrared spectroscopy, and its result is as follows (KBr): υ (cm -1 ): 3315, 2983, 2758, 1703, 16...

Embodiment 2

[0040] Synthesis of polyimide

[0041] 1g4,4'-diaminodiphenyl ether (ODA) is added into a three-necked flask, poured into an appropriate amount of dimethylacetamide (DMAc) solvent, fully stirred to fully dissolve ODA in DMAc, and then added biphenyltetracarboxylic dianhydride ( BPDA) 1.5g, that is, the molar ratio of ODA to BPDA is 1:1, stirred at room temperature for 6-8 hours, the resulting polyimide prepolymer - polyamic acid (PAA). On a clean substrate, use a threaded coating rod or a spin coater to coat the film (the spin coating speed is 2000rpm), put it in a vacuum oven, and use the gradient heating imidization method, that is, 100 ° C for 1 hour, 200 ° C for 1 hour , 300° C. for 0.5 hours to convert PAA into a polyimide film (abbreviated as PI), which has a refractive index of 1.727 at 633 nm at room temperature. (see attached figure 1 )

[0042] Infrared spectrum characterization, the results are as follows (KBr): υ(cm -1 ): 3315, 1720, 1605, 1499, 1363, 1204, 110...

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Abstract

The invention relates to a modified polyimide film. The modified polyimide film is prepared by the steps of: placing carbon black subjected to organification treatment, a dianhydride monomer, a diamine monomer and an organic solvent in a reactor provided with a mixing device, evenly stirring and mixing at the temperature not higher than 40 DEG C to obtain a mixture, wherein the carbon black subjected to organification treatment relates to carrying out grafting and / or cladding on the surface of the carbon black with -COOH, -OH, -COX or / and amino functional groups, or relates to the carbon black contains organic compounds of the -COOH, -OH, -COX or / and amino functional groups, and X is halogen; and spreading the mixture evenly on a substrate; and finally solidifying in the presence of vacuum at 60 DEG C-350 DEG C in a gradient temperature rising way. Compared with the traditional polyimide film, the modified polyimide film has improvements not only in optical property (refractive index), but also in mechanical property and thermal stability.

Description

technical field [0001] The invention relates to a modified polyimide film, in particular to a polyimide film modified by organically treated carbon black. Background technique [0002] Polyimide (polyimide, PI), is a main chain structure unit containing imide group of synthetic resins. [0003] Polyimide is a typical high refractive index film, such as standard polyimide [pyromellitic dianhydride (PMDA) - diaminodiphenyl ether (ODA)] at 25 ° C, 633nm The refractive index is as high as 1.695. In addition, the rigid imide ring structure of polyimide not only endows it with high refractive index, but also endows it with high heat resistance stability, high mechanical properties and dielectric properties. The excellent comprehensive properties of polyimide make it Widely used in optical devices. However, the standard polyimide usually has a darker color, the birefringence of the film is larger, and the refractive index is still difficult to meet the requirements of some opt...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08J5/18C08L79/08
Inventor 李秋影吴驰飞薛鹏飞郭卫红许海燕鲍宇彬王纪彬周麒麟洪娟
Owner EAST CHINA UNIV OF SCI & TECH
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