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Preparation method of superparamagnetic polyimide composite film

A technology of superparamagnetic and composite films, which is applied in the field of preparation of superparamagnetic polyimide composite films, can solve the problems of low saturation magnetization, poor uniformity, irregular particle shape, etc., and achieve high magnetic saturation, distribution uniform effect

Pending Publication Date: 2021-12-31
LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fe used in this method 3 o 4 Magnetic nanoparticles are obtained by co-precipitation method, which has the disadvantages of irregular particle shape, poor uniformity, and low saturation magnetization.

Method used

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  • Preparation method of superparamagnetic polyimide composite film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of a superparamagnetic polyimide composite film, comprising the following steps:

[0025] Step 1. Add 1.5g iron acetylacetonate, 10g 1,2-hexadecyl glycol, 0.1g oleic acid, 0.1g oleylamine and 300g benzyl ether into the reactor and heat at a heating rate of 3.3°C / min to 200°C, keep it warm for 2 hours, then heat to the boiling point of benzyl ether, that is, reflux at 298°C for 1 hour, after the reaction is completed, cool to room temperature, add absolute ethanol to the reaction solution to obtain Fe 3 o 4 For magnetic nanoparticle precipitation, the precipitate was centrifuged at 3000rpm for 10min to remove the upper layer solution; to obtain Fe 3 o 4 magnetic nanoparticles;

[0026] Step two, 6g Fe 3 o 4 Magnetic nanoparticles were dispersed in 30mL of n-hexane, then 0.15g of 4-aminophenyltrimethoxysilane and 0.003g of glacial acetic acid were added dropwise and shaken for 72 hours to obtain a precipitate; the precipitate was separated by a m...

Embodiment 2

[0030] A preparation method of a superparamagnetic polyimide composite film, comprising the following steps:

[0031] Step 1. Add 1.5g iron acetylacetonate, 10g 1,2-hexadecyl glycol, 0.1g oleic acid, 0.1g oleylamine and 300g benzyl ether into the reactor and heat at a heating rate of 3.3°C / min to 200°C, keep it warm for 2 hours, then heat to the boiling point of benzyl ether, that is, reflux at 298°C for 1 hour, after the reaction is completed, cool to room temperature, add absolute ethanol to the reaction solution to obtain Fe 3 o4 For magnetic nanoparticle precipitation, the precipitate was centrifuged at 3000rpm for 10min to remove the upper layer solution; to obtain Fe 3 o 4 Magnetic nanoparticles; Fe obtained by low-temperature plasma 3 o 4 Magnetic nanoparticles are processed, the process is: the Fe 3 o 4 The magnetic nanoparticles are placed in the low-temperature plasma treatment reaction chamber, and the vacuum pump is turned on. After the vacuum degree in the ch...

Embodiment 3

[0036] A preparation method of a superparamagnetic polyimide composite film, comprising the following steps:

[0037] Step 1. Add 1.5g iron acetylacetonate, 10g 1,2-hexadecyl glycol, 0.1g oleic acid, 0.1g oleylamine and 300g benzyl ether into the reactor and heat at a heating rate of 3.3°C / min to 200°C, keep it warm for 2 hours, then heat to the boiling point of benzyl ether, that is, reflux at 298°C for 1 hour, after the reaction is completed, cool to room temperature, add absolute ethanol to the reaction solution to obtain Fe 3 o 4 For magnetic nanoparticle precipitation, the precipitate was centrifuged at 3000rpm for 10min to remove the upper layer solution; to obtain Fe 3 o 4 Magnetic nanoparticles; Fe obtained by low-temperature plasma 3 o 4 Magnetic nanoparticles are processed, the process is: the Fe 3 o 4 The magnetic nanoparticles are placed in the low-temperature plasma treatment reaction chamber, and the vacuum pump is turned on. After the vacuum degree in the ...

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Abstract

The invention discloses a preparation method of a superparamagnetic polyimide composite film. The preparation method comprises the following steps: preparing Fe3O4 magnetic nanoparticles; dispersing Fe3O4 magnetic nanoparticles in normal hexane, then dropwise adding a silane coupling agent and glacial acetic acid, and oscillating the mixture for 72 hours to obtain a precipitate; separating the precipitate by using a magnet, repeatedly cleaning the precipitate by using an n-hexane / pentane mixed solvent to obtain silane coupling agent modified Fe3O4 magnetic nanoparticles, and ultrasonically dispersing the Fe3O4 magnetic nanoparticles in DMF to obtain a magnetic nanoparticle DMF phase dispersion liquid; adding biphenyl tetracarboxylic acid and p-phenylenediamine into the DMF phase dispersion liquid of the magnetic nanoparticles to obtain a superparamagnetic polyamide acid solution; and preparing the superparamagnetic polyimide composite film from the superparamagnetic polyamide acid solution through a Czochralski method and high-temperature imidization. The magnetic nanoparticles adopted by the superparamagnetic polyimide composite film are obtained through a high-temperature decomposition method; compared with other methods, the superparamagnetic polyimide composite film has high magnetic saturation intensity.

Description

technical field [0001] The invention relates to a preparation method of a superparamagnetic polyimide composite film. Background technique [0002] Polyimide film is a kind of high-performance polymer film characterized by imide structure. It has excellent heat resistance, chemical stability, radiation resistance, mechanical strength and electrical properties. It is widely used in electronic information, aerospace, etc. The field has a very wide range of applications. Especially in the field of electromagnetic shielding, the polyimide film compounded with superparamagnetic materials has shown good application value due to its characteristics of easy processing and mass production. [0003] China Invention Patent Application No. 201810849031.2 discloses a method for preparing a magnetic polyimide composite film. The method first synthesizes 2,6-diamino-13,14,15,16-tetrachlorotriptycene, and then synthesizes porous polyimide containing triptycene structure with hexafluorodia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G73/10C08L79/08C08K9/06C08K3/22
CPCC08J5/18C08G73/1067C08G73/1007C08K9/06C08K3/22C08J2379/08C08K2003/2275C08K2201/01
Inventor 朱方华王宇光万翔宇晏良宏徐嘉靖李娃
Owner LASER FUSION RES CENT CHINA ACAD OF ENG PHYSICS
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