Ultralow dielectric constant film with sandwich structure and preparation method thereof
An ultra-low dielectric constant, sandwich technology, applied in the field of ultra-low dielectric constant film and its preparation, can solve problems such as low dielectric constant, and achieve the effects of low dielectric constant, excellent heat resistance, and easy realization
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[0035] b) The preparation method of mesoporous molecular sieve (MCM-41) is as follows:
[0036] Dissolve 120g of cetyltrimethylammonium bromide in 2L of deionized water, stir at room temperature for 30min to make it fully dissolved; add 2.5L of absolute ethanol and 680g of ammonia (25%), stir for 25min; then add 180ml of normal Ethyl silicate, stirring at room temperature for 6 hours; then static aging at room temperature for 1 hour. Suction filtration, washing to neutrality, and drying to obtain raw powder; the raw powder is placed in a muffle furnace, and calcined at 1°C / min to 580°C for 6 hours in an air atmosphere to obtain MCM-41.
[0037] c) Organic monomer: pyromellitic dianhydride (PMDA): Sinopharm Chemical Reagent Co., Ltd.; 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA): SIGMA-ALDRICH China Co., Ltd. ; 4,4'-Diaminodiphenyl ether (ODA): Sinopharm Chemical Reagent Co., Ltd.; p-phenylenediamine (p-PDA): Sinopharm Chemical Reagent Co., Ltd.;
[0038] d) Solvent: N,N...
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[0043] Example 1
[0044] Synthesis of polyamic acid solution for dense layer preparation:
[0045] Under the protection of nitrogen, after dissolving 0.9649g ODA in 50ml NMP, slowly adding 1.5535g BTDA, and reacting at 20°C for 15 hours after the addition to obtain a polyamic acid solution with a solid content of 0.05g / ml.
[0046] Preparation of polyamic acid dense base film:
[0047] Drop the above 6ml polyamic acid solution on a horizontally placed glass plate and cast to form a film; remove the solvent at 60°C for more than 18 hours. Then immerse it in hot water and cook for 5-10 minutes, and scrape it off gently to get a dense polyamic acid film.
[0048] Synthesis of polyamic acid solution for electrospun membrane preparation:
[0049] Under the protection of nitrogen, after dissolving 3.9752g ODA in 58ml DMF, slowly adding 6.5248g BTDA, and reacting at 15°C for 20 hours after addition, to obtain a polyamic acid solution with a solid content of 0.18g / ml.
[0050] Preparation of el...
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[0056] Example 2
[0057] Synthesis of polyamic acid / OAPS hybrid solution for dense layer preparation:
[0058] 1) Dissolve 0.0233g OAPS in 40ml DMSO;
[0059] 2) Under the protection of nitrogen, add 0.5516g ODA to the above dispersion; after the ODA is completely dissolved, slowly add 0.6129g PMDA, and react at 20°C for 18 hours after the addition to obtain a solid content of 0.03g / ml and an OAPS content of 2. % Homogeneous polyamic acid / OAPS hybrid solution.
[0060] Preparation of polyamic acid / OAPS hybrid dense base film:
[0061] Drop the above 6ml polyamic acid / OAPS hybrid solution on a horizontally placed glass plate and cast to form a film; remove the solvent at 60°C for more than 18 hours. Then immerse it in hot water and cook for 5-10 minutes, and gently scrape to obtain a dense polyamic acid / OAPS hybrid film.
[0062] Synthesis of polyamic acid / OAPS hybrid solution for electrospun membrane preparation:
[0063] 1) Dissolve 0.5250g OAPS in 79ml DMF;
[0064] 2) Under the prote...
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