Preparation method of doped polyimide composite film for FCCL (flexible copper clad laminate)

A polyimide and composite film technology, which is applied in the field of preparation of doped polyimide composite films, can solve the problems of prolonging the curing time, increasing the curing temperature, and differential thermal processing performance, so as to achieve easy control of the preparation process , lower thermal expansion coefficient, good modification effect

Inactive Publication Date: 2014-10-15
LAIWU ZHONGTIAN INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Russian Bershtein and others studied the inorganic doping material SiO 2 For PI / SiO 2 The influence of molecular dynamics and thermal stability of the hybrid film, the results show that with SiO 2 The increase of the content of the molecular chain decreases the molecular chain mobility, which is manifested by the decrease of the thermal expansion coefficient of the hybrid film; but doped SiO 2 The hybrid film has poor thermal processability
Ker-Ming Chen prepared high-strength polyimide films by curing the copolymeric polymer system p-phenylenediamine / 4,4'-diaminodiphenyl ether / biphenyltetracarboxylic dianhydride at different temperatures. To prepare films with strong crystalline structures or interchain reactions and high bulk density with high mechanical properties, the curing temperature should be increased and the curing time should be prolonged; however, this treatment process requires more stringent equipment requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 500mL of DMAc solution to a three-necked flask, add 40.048g of 4,4'-diaminodiphenyl ether to dissolve it completely, then add 4.1836g of zirconium molybdate powder to the solution, and treat it with a high-speed shear disperser for 25min After switching to electromagnetic stirring to disperse evenly, add PMDA with a molar ratio of 1:1 to 4,4'-diaminodiphenyl ether into the mixing system in 3 times, and ensure that the added PMDA is completely reaction. Raise the temperature to 50°C and react for about 9 hours to prepare doped ZrMo 2 o 8 polyamic acid (PAA) resin.

[0022] Put the obtained PAA resin in a vacuum drying oven for 120 minutes to remove air bubbles, then pour it on a clean glass plate and scrape it to form a resin layer, dry it at 120°C for 1 hour to form a film, remove it and fix it on the iron frame , baked at 140°C, 180°C, 220°C, 260°C, and 380°C for 1 hour, and imidized at 400°C to prepare doped ZrMo with low thermal expansion coefficient 2 o 8 / ...

Embodiment 2

[0025] Add 500mL of NMP solution into a three-necked flask, add 40.048g of 4,4'-diaminodiphenyl ether into it to dissolve it completely, then add 12.5508g of zirconium molybdate powder to the solution, and treat it with a high-speed shear disperser for 25min After switching to electromagnetic stirring to disperse evenly, add PMDA with a molar ratio of 1:1 to 4,4'-diaminodiphenyl ether into the mixing system in 3 times, and ensure that the added PMDA is completely reaction. Raise the temperature to 45°C and react for about 10 hours to prepare doped ZrMo 2 o 8 polyamic acid (PAA) resin.

[0026] Put the obtained PAA resin in a vacuum drying oven for 120 minutes to remove air bubbles, then pour it on a clean glass plate and scrape it to form a resin layer, dry it at 100°C for 1 hour to form a film, remove it and fix it on the iron frame , baked at 140°C, 180°C, 220°C, 260°C, and 380°C for 1 hour, and imidized at 320°C to prepare doped ZrMo with low thermal expansion coefficien...

Embodiment 3

[0029] In a three-necked flask, add 500mL of DMAc solution, add 40.048g of benzidinediamine to make it completely dissolved, then add 8.3672g of zirconium molybdate powder to the solution, and switch to electromagnetic stirring after 25min with a high-speed shear disperser. After making it dispersed evenly, add BPDA with a molar ratio of 1:1 to the benzidinediamine into the mixing system in 3 times, and ensure that the BPDA added is completely reacted each time. Raise the temperature to 55°C and react for about 8 hours to prepare doped ZrMo 2 o 8 polyamic acid (PAA) resin.

[0030] Put the obtained PAA resin in a vacuum drying oven for 120 minutes to remove air bubbles, then pour it on a clean glass plate and scrape it to form a resin layer, dry it at 180°C for 1 hour to form a film, remove it and fix it on the iron frame , baked at 140°C, 180°C, 220°C, 260°C, and 380°C for 1 hour, and imidized at 450°C to prepare doped ZrMo with low thermal expansion coefficient 2 o 8 / P...

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Abstract

The invention relates to a preparation method of doped polyimide composite film for FCCL (flexible copper clad laminate). The specific process of the preparation method is as follows: dissolving a certain amount of diamine monomer in an organic solvent, fully stirring to dissolve; adding doping reagent zirconium molybdate, using a high-speed shear dispersing device for uniformly stirring to disperse; and then adding dianhydride with the same molar ratio of the diamine into mixed system for a plurality of times to ensure the dianhydride added for each time is fully reacted, polymerizing, and performing thermal imidization processing to prepare the ZrMo2O8 / PI (polyimide) composite film. The preparation process is simple, the obtained composite film product is low in thermal expansion coefficient and has good application effect in the FCCL.

Description

technical field [0001] The invention belongs to the field of composite film preparation, and in particular relates to a method for preparing a doped polyimide composite film. The composite film can be used as an electronic packaging material and is widely used in the fields of FPC, FCCL and other electronic components. Background technique [0002] With the continuous development of the integrated circuit industry, high-performance electronic packaging technology has formed a corresponding high-tech industry. The miniaturization trend of electronic equipment drives FPC technology to develop in the direction of high efficiency and high density. High density means fine lines, tiny holes and multi-layer wiring, which requires films to have low thermal expansion coefficient, high reliability, high strength and good processing performance, etc. Generally speaking, copper foil is bonded with multi-layer polyimide (PI) film to make FCCL, which has undergone multiple thermal cycles...

Claims

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Application Information

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IPC IPC(8): C08J5/18C08L79/08C08K3/24C08G73/10
Inventor 李兰玉王文晓祝春才何美玲
Owner LAIWU ZHONGTIAN INSULATING MATERIAL
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