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, achieve low dielectric constant, excellent heat resistance, and easy to achieve
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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 fully dissolve; add 2.5L of absolute ethanol and 680g of ammonia water (25%), stir for 25min; add 180ml of normal Ethyl silicate, stirred at room temperature for 6h; then aged at room temperature for 1 hour. Suction filtration, washing until neutral, and drying to obtain the original powder; put the original powder in a muffler furnace, and roast at 1°C / min to 580°C for 6 hours under an air atmosphere to obtain MCM-41.
[0037] c) Organic monomers: pyromellitic dianhydride (PMDA): Sinopharm Chemical Reagent Co., Ltd.; 3,3',4,4'-benzophenone tetracarboxylic 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-di...
Embodiment 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 add 1.5535gBTDA, after the addition, react at 20°C for 15 hours to obtain a polyamic acid solution with a solid content of 0.05g / ml.
[0046] Preparation of polyamic acid dense base film:
[0047] Drop 6ml of the above polyamic acid solution onto a glass plate placed horizontally, 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 add 6.5248gBTDA, after the addition, react at 15°C for 20 hours to obtain a polyamic acid solution with a solid content of 0.18g / ml.
[0050] Preparation of electrospun membra...
Embodiment 2
[0057] Synthesis of polyamic acid / OAPS hybrid solution for dense layer preparation:
[0058] 1) Dissolve 0.0233gOAPS in 40mlDMSO;
[0059] 2) Under the protection of nitrogen, add 0.5516g ODA to the above dispersion liquid; 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 % of a homogeneous polyamic acid / OAPS hybrid solution.
[0060] Preparation of polyamic acid / OAPS hybrid dense base film:
[0061] Drop 6ml of the above-mentioned polyamic acid / OAPS hybrid solution on a glass plate placed horizontally, 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 / OAPS hybrid film.
[0062] Synthesis of polyamic acid / OAPS hybrid solution for electrospun membrane preparation:
[0063] 1) Dissolve 0.5250g OAPS in 79ml DMF;
...
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