Novel electronic-grade polyimide film with low linear expansion coefficient and production method thereof
A polyimide film, low linear expansion coefficient technology, applied in the low linear expansion coefficient polyimide film and its production field, can solve the problem that can not meet the needs of high-end electronic products, the polyimide linear expansion coefficient is large, High dimensional stability and other issues, to achieve the effects of large-scale industrial production, low linear expansion coefficient and low cost
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Embodiment 1
[0062] Put 500 liters of DMF into the dissolving kettle, add 1.00 molar ratio of ODA, start the mixer to stir and dissolve, the dissolution time is 1 hour, after the diamine monomer is completely dissolved in the polar solvent, stop the stirring, and use compressed air to separate the diamine The body solution is pressed into the stainless steel polymerization reactor through the filter, the mixer is started, the cooling water is passed through, and then the dianhydride monomers (PMDA, BPDA, BTDA and their combinations) with a total molar ratio of 1.010~1.015 are gradually added in 8 times . For the 1st to 4th times, the amount of dianhydride added is controlled at equal and uniform intervals. The first 4 times add 50wt% of the total amount of dianhydride. From the 5th to 8th times, each addition is 50wt% of the total balance. Put in, and check the resin viscosity after 5-10 minutes of stirring and reaction after each feeding. When the polyamic acid resin glue with a solid cont...
Embodiment 2
[0066] Refer to the solution polycondensation method of Example 1, using DMF as the solvent, polycondensation of the dianhydride and diamine in the same molar ratio to obtain a polyamic acid solution with a solid content of 15-20%, which is filtered and vacuum degassed. The mixed polyamic acid solution is cast on an endless steel belt through an extrusion die to form a film, which is chemically imidized to form a gel film with a solid content of 22.5% to 55%, and then the steel belt is peeled off by a peeling roller and sent by a silicone roller To the longitudinal stretching machine and the transverse stretching machine, the biaxial stretching is carried out at a stretching ratio of 1.10 to 1.35 at a temperature of 125~185℃, and the biaxial stretching film is then subjected to a high temperature of 15min~25min in an infrared box at 350~450℃ Fully imidized, heat setting in a high temperature box at 250-300℃ for 5min-8min, corona surface modification, natural cooling, edge trimmi...
Embodiment 3
[0073] Referring to Example 1, a multi-component blended polyamic acid was synthesized by a stepwise feeding method.
[0074] Anhydrous N,N'-dimethylformamide 85% (parts by weight) and 15% (parts by weight) of anhydrous N,N'-dimethylformamide purified and pre-measured in a solvent tank with a mass of 4 times the total amount of dianhydride and diamine monomers ) Put the mixed solvent into the dissolving kettle, put 108kg of high-purity p-phenylenediamine and 367kg of APDS into the dissolving kettle through the automatic metering system, start the mixer to stir and dissolve, the dissolution time is not less than 1.0 hour, and the diamine monomer is completely dissolved After the polar solvent, stop stirring, use compressed air to press the diamine monomer solution into the stainless steel polymerization reactor through the filter, start its agitator, pass cooling water, and then gradually add the total amount in 8 batches under stirring 294kg of pyromellitic dianhydride, control t...
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