Method of forming a nanoporous dielectric film
A nanoporous, pore-forming technology, applied in the fields of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve problems such as difficulties
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Embodiment 1
[0096] Embodiment 1 - the method for producing chemical formula I monomer
[0097] A. Synthesis of ethyl 4-bromophenyl acetate
[0098] A solution of 63 g (0.29 mol) of 4-bromophenylacetic acid and 50 ml of concentrated sulfuric acid in 500 ml of pure ethanol was refluxed for 8 hours and then left to stand overnight. After pouring 600 g of ice, the mixture was extracted with ether / hexane. The ether extract was washed well with water and sodium bicarbonate solution, then dried over anhydrous sodium sulfate. Removal of the solvent by rotary evaporation yielded 57 g (0.24 mol, 80% isolated yield) of an oil which crystallized on cooling. Filtration and washing with hexanes yielded pure product.
[0099] B. Synthesis of 1,3-bis(4-bromophenyl)-2-propanone
[0100] To a slurry of sodium hydride (9.17 g, 0.23 mol) in 50 ml of toluene was added dropwise ethyl 4-phenylbromoacetate (50 g, 0.21 mol) in toluene (50 ml) at 30-32°C solution. After the addition was complete, the reactio...
Embodiment 2
[0108] Embodiment 2 - the method for producing chemical formula XVI monomer
[0109] A. Synthesis of 4-bromophenylacetyl chloride
[0110] 4-Bromophenylacetic acid (99.5 g, 0.46 mol) and N,N-dimethylformamide (2 mL) were added to a pre-dried one-liter glass one-neck round-bottom Schlenk reactor under dry nitrogen , the reactor contained a pre-dried magnetic stir bar. After sealing under dry nitrogen, the reactor was placed above a Schlenk tube under a slightly positive nitrogen pressure. Thionyl chloride (300 mL) was added under dry nitrogen to a pre-dried glass addition funnel fitted with a Schlenk adapter, which was then sealed under dry nitrogen and placed on a Schlenk tube. The reactor and addition funnel were connected under a flow of dynamic nitrogen before all the thionyl chloride was added to the stirred reactor. Nitrogen flow was maintained into the Schlenk reactor while exhaust gas from the reaction entered the scrubber system through the Schlenk adapter on the ad...
Embodiment 3-
[0120] Example 3 - Method of Producing Porous Membrane
[0121] Add 3.0 g of chemical formula I monomer, 1.50 g of linear polystyrene (Mn=1,900 g / mole, Mw / Mn=1.10, purchased from Scientific Polymer Products, Inc. .) and 9.0 grams of gamma-butyrolactone (GBL). The synthesis mixture was purged under nitrogen for 15 minutes and then heated to 180° C. for 4.0 hours using an oil bath under nitrogen. The mixture was then cooled to 145°C and diluted with 8.0 g of cyclohexanone. The mixture was further cooled to room temperature to give a polymer mixture (21% by weight) in GBL / cyclohexanone. GPC indicated that the formulation had a molecular weight of 43,000 g / mole (Mw) and a degree of polymerization distribution of 4.7.
[0122] This mixture was applied to a silicon wafer and a ~0.9 micron thick film was formed by spin-coating casting. The film was baked on an MTI hotplate at 150°C for 2 minutes, and then the coated sheet was transferred to a vacuum oven. The oven temperature wa...
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