Defect reduction methods and composition for via formation in directed self-assembly patterning
A technology of hydrophobic polymers and block copolymers, applied in the fields of technology for producing decorative surface effects, decorative art, gaseous chemical plating, etc., can solve problems such as undiscussed defects
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Embodiment 1
[0122] Synthesis Example 1: Synthesis of an azo initiator with phosphonate side groups
[0123] (1) 4,4'-Azobis(4-cyanovaleryl chloride) as a mixture of isomers: All procedures were performed under nitrogen atmosphere. Prepare 70 g of PCl in a round bottom flask with a mechanical stirrer 5 Suspension in about 240 ml of dichloromethane. To this suspension were added portionwise 9.1 g of 4,4'-azobis(4-cyanovaleric acid) within 25 minutes. The mixture was stirred at 0-2°C for 2 hours, then for 40 hours while heating to 16°C. Filter off excess phosphorus pentachloride solids using CH 2 Cl 2 (2x10ml) wash. The resulting solution was concentrated at room temperature using a rotary evaporator to obtain 115 g of a colorless liquid. The material was then placed in a -20°C freezer for 4 hours. The cold solution was poured into 200ml hexane with good stirring, the colorless solid was filtered and washed well with hexane. Yield: 7.3g (70.8%); m.p.75-77°C; 1 H NMR (CDCl 3 ,δppm) ...
Embodiment 2
[0126] Synthesis Example 2: Synthesis of Polystyrene Brush Precursors with Phosphonate End Groups
[0127] 1.7234 g (1.84 mmol) of the azo initiator prepared in Example 1 (3) above dissolved in 60 ml of 2-butanone was prepared in a 250 ml flask equipped with a magnetic stirrer, water condenser and gas bubbler , 44.779g (0.43mol) solution composed of styrene. Nitrogen was bubbled through the solution for 45 minutes, and the mixture was heated to 80° C. for 15.5 hours while stirring. The reaction mixture was cooled to room temperature and the solution was poured slowly into 1.8 L MeOH with stirring. The polymer was isolated by filtration, dried (60 °C) and purified by reprecipitation from 95 ml THF solution into 1.3 L methanol, washed with methanol and dried in a vacuum oven at 60 °C until a constant weight of 20.4 g, yield: 43.9%. Mn 23086g / mol; M w 40616 g / mol; PD 1.76. 1 H NMR (CDCl 3 ,δppm): 3.58-3.4(m,-CH 2 -N),4.18-3.98(m,CH 3 -C H 2 -O-P);
Embodiment 3
[0128] Synthesis Example 3: Synthesis of an azo initiator with hydroxyl side groups
[0129] (1) A solution of tetramethylammonium pentahydrate was prepared by dissolving 63 g of this material in (0.348 mol) 100 g of methanol. The solution was slowly added to a solution of 48.72 g (0.174 mol) of 4,4'-azobis(4-cyanovaleric acid) suspended in 100 g of methanol at a rate of addition with stirring so that the reaction temperature did not rise above 40 ℃. The reaction mixture was stirred for an additional hour after the addition was complete. After this time most of the methanol was stripped from the reaction mixture using a rotary evaporator at room temperature. The concentrated reaction mixture was then poured into a flask containing diethyl ether so an oily layer precipitated at the bottom of the flask. The supernatant ether was then decanted and an oily residue was retained. The residue was washed by adding more diethyl ether to the flask containing the oily residue with st...
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