A kind of polyimide multilayer composite film with high modulus and low thermal expansion coefficient and its preparation method and application
A low thermal expansion coefficient, polyimide layer technology, applied in the direction of coating, etc., can solve the problems that affect the final film performance, decrease the toughness of the composite film, increase the difficulty of blending, etc., achieve low thermal expansion coefficient, low cost, high modulus effect
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[0045] The preparation method of the present invention will be further described in detail in conjunction with specific examples below. It should be understood that the following examples are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by the present invention.
[0046] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents and materials used in the following examples can be obtained from commercial sources unless otherwise specified.
[0047] The polyamic acid solutions in the following examples can be prepared as follows, and the specific steps are as follows: under the protection of nitrogen, first dissolve the diamine monomer in an organic solvent to obtain a homogeneous transp...
Embodiment 1
[0048] Embodiment 1, preparation PMDA-ODA / PMDA-PDA / PMDA-ODA system three-layer composite film
[0049] 1) The pyromellitic dianhydride-4,4'-diaminodiphenyl ether (PMDA-ODA) / NMP solution with a mass fraction of 20wt% is evenly coated on a glass plate, and placed in a vacuum drying oven to The temperature was raised to 150°C at a rate of 2°C / min, and then the temperature was naturally cooled to room temperature before being taken out. The thickness of the obtained PMDA-ODA film was about 20 μm.
[0050] 2) The pyromellitic dianhydride-p-phenylenediamine (PMDA-PDA) / NMP solution with a mass fraction of 20wt% is uniformly coated on the PMDA-ODA film prepared in the previous step, and after standing at room temperature for 2h, place In a vacuum drying oven, the temperature was raised to 120°C at a rate of 2°C / min, and then the temperature was naturally cooled to room temperature and taken out. The thickness of the obtained PMDA-PDA film was about 20 μm.
[0051] 3) Evenly coat the ...
Embodiment 2
[0064] Embodiment 2, the preparation upper and lower floors are polyimide (PI), and the middle layer is a three-layer composite film (s-PI-CF) of carbon fiber reinforced polyimide (PI-CF)
[0065] 1) Evenly coat the PMDA-ODA / NMP solution with a mass fraction of 20wt% on a glass plate, place in a vacuum drying oven, heat up to 180°C at a rate of 2°C / min, and then take it out after naturally cooling to room temperature, The thickness of the obtained PMDA-ODA film is about 10 μm.
[0066] 2) The PMDA-ODA / CF blend solution (the mass ratio of CF and polyamic acid is 0.05:0.95) with a mass fraction of 20wt% is evenly coated on the PMDA-ODA film prepared in the previous step, and placed in a vacuum drying oven , the temperature was raised to 180 °C at a rate of 2 °C / min, and then the temperature was naturally cooled to room temperature and taken out. The thickness of the obtained PMDA-ODA / CF film was about 10 μm.
[0067]3) Coat the PMDA-ODA / NMP solution with a mass fraction of 20wt...
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