Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof

A polyimide film, low linear expansion coefficient technology, applied in the field of polymer engineering materials, can solve problems such as unsolved problems, and achieve the effects of high industrial application value, excellent adhesion performance, and excellent reinforcement effect.

Active Publication Date: 2014-01-22
宏威高新材料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Domestic and foreign patents or public documents have also carried out a single study on the above method, because it failed to comprehensively consider the special comprehensive performance requirements of modern information technology for flexible printed circuit boards for high-end polyimide film substrates, especially failed to solve Very low coefficient of linear expansion and excellent film-forming properties of polyamic acid, as well as the requirements of flexibility, adhesion, moisture expansion resistance and high mechanical properties of polyimide film materials

Method used

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  • Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof
  • Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof
  • Novel electronic-grade polyimide film with low linear expansion coefficient and manufacturing method thereof

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preparation example Construction

[0042] A method for preparing a polyimide film with a low coefficient of linear expansion, comprising the following contents and process steps:

[0043] (1) Synthesis of step-by-step condensation polyamic acid resin: the present invention uses more than two kinds of diamine monomers and tetracarboxylic dianhydride as raw materials, and adopts the "interpenetrating compound in polymer kettle" technology of multi-stage step-by-step polymerization Synthesis of multi-component block copolymerized polyamic acid resin. That is, the polyamic acid A with the design viscosity is first synthesized by the general polyamic acid synthesis technology, and then another or more diamines and dianhydride monomers are added according to the design molar ratio, and the reaction is carried out for a period of time to obtain the original polyamide A-B-C-… type large block copolymerized polyamic acid in which polyamic acid B is inserted into the molecular chain of acid A. The outstanding advantage ...

Embodiment 1

[0065] Put 500 liters of DMF into the dissolution tank, add 1.00 molar ratio of ODA, start the mixer to stir and dissolve, and the dissolution time is 1 hour. After the diamine monomer is completely dissolved in the polar solvent, stop stirring, and use compressed air to dissolve the diamine monomer. The body solution is pressed into the stainless steel polymerization reaction kettle through the filter, the mixer is started, the cooling water is passed, and then the dianhydride monomer (PMDA, BPDA, BTDA and its composition) is gradually added in 8 times with a total molar ratio of 1.010 to 1.015. . From the 1st to 4th times, the amount of dianhydride added is controlled in equal amounts and at even intervals. A total of 50wt% of the total amount of dianhydride is added in the first 4 times. From the 5th to 8th times, each addition is 50wt% of the total amount of the remaining amount. Putting in, checking the viscosity of the resin after stirring and reacting for 5-10 minutes e...

Embodiment 2

[0068] Example 2 Synthesize the polyamic acid by the block copolymerization of multiple rigid chain acid anhydrides and two or more diamines of ether bonds or siloxane bonds by gradually adding diamine and dianhydride raw materials

[0069] First, the polar aprotic solvent (DMF, DMAc or NMP or any combination of any proportion) that is purified and pre-measured in the solvent tank and whose mass is 3.5 to 7 times the total amount of dianhydride and diamine monomers is put into the dissolution tank 0.50-0.70 molar ratio of ODA and 0.25-0.20 molar ratio of 1,3-bis(3-aminopropyl)tetramethyldisiloxane (APDS) were put into it through the automatic metering system, and the mixer was started to stir and dissolve , the dissolution time is not less than 1.5 hours. After the diamine monomer is completely dissolved in the polar solvent, stop stirring, and add 0.65-0.75 molar ratio of PMDA to the polymerization kettle in 5 batches at intervals of 10-30 minutes. After completion, continue ...

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Abstract

The invention relates to a manufacturing method of an electronic-grade polyimide film with low linear expansion coefficient. The method is characterized by comprising the steps that (1) the step-by-step condensation polymerization technology or the blending compounding technology is used for obtaining two or more polyamide acid glue solutions comprising rigid structures and soft structures at the same time and are different in rigidity and softness; (2) ultrafine inorganic whiskers, like zinc oxide whiskers, silicon carbide whiskers and zirconium tungstate whiskers, which are subjected to surface organic modification already and/or nanoparticle materials are smashed and cavitated through high-energy-density supersonic waves, and then the functional fillers are compounded with polybasic polyamide acid in an in-situ micro-nano mode; (3) the compounded glue solutions are subjected to filtration, vacuum defoamation, extrusion casting filming, chemical amidization or thermal amidization, infrared complete amidization, high-temperature thermal forming processing, corona processing and a reeling process, and therefore the electronic-grade polyimide film with the thickness being 7.5-125 micrometers, the linear expansion coefficient being 5-18ppm/DEG C, and good physical mechanical performance is obtained.

Description

technical field [0001] The invention relates to a polyimide film with a low linear expansion coefficient that mainly meets the requirements of high-end flexible printed circuit boards and a production method thereof, in particular to a polyimide with a low linear expansion coefficient, which belongs to the technical field of polymer engineering materials. Background technique [0002] Polyimide (PI) refers to a class of aromatic heterocyclic polymers containing imide rings in the main chain. It has excellent mechanical, dielectric, radiation resistance, and corrosion resistance at high temperatures. It is an organic polymer One of the materials with the best comprehensive properties among materials, known as the "Pearl in the Crown" of high-tech materials and the "expert" in solving microelectronics technologies such as VLSI in the 21st century, it is used in aerospace, electronic information, automobiles Industry and other fields have a broad application space. [0003] Po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L79/08C08G73/10C08K9/06C08K9/04C08K7/10C08K7/08C08K7/06C08K3/36C08K3/22C08K3/24
Inventor 李晓敏袁萍黄渝鸿李旺曹君袁彬彬杨帆陈凤阳龑黄小诚李涛韩青霞
Owner 宏威高新材料有限公司
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