Double-bond-modified polyhedral oligomeric silsesquioxane and photoresist composition thereof
A technology of silsesquioxane and composition, which is applied in the field of double bond modified cage-type silsesquioxane and its preparation, can solve the problems of large internal stress, restrict development, weaken the adhesion of the system, and achieve high adhesion. The effect of focusing on, solving volume shrinkage and good thermal stability
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Embodiment 1
[0049] A preparation method containing double bond modified cage silsesquioxane, comprising the following steps:
[0050] Weigh 1 mol of cage-type silsesquioxane shown in formula I, 3 mol of triethylamine, and 5 mol of xylene solution in a flask, weigh 1.2 mol of acryloyl chloride and add it to a spherical dropping funnel, and place the flask in a water bath Add ice to the water bath, drop acryloyl chloride into the flask at a rate of one drop per second under the ice bath, and stir magnetically; add 500ppm of polymerization inhibitor hydroxyanisole, and stir the reaction for 1h under the ice bath; after the reaction, Then heat up to 20°C and react for 30h; filter the obtained product, then wash with saturated sodium bicarbonate solution for 3 times and separate liquid, water liquid, remove water with anhydrous sodium sulfate, remove solvent by rotary evaporation, and then dry in a vacuum oven at 20°C Drying under the condition for 12 hours, the product containing double bond-...
Embodiment 2
[0056] A preparation method containing double bond modified cage silsesquioxane, comprising the following steps:
[0057] Weigh 1 mol of cage-type silsesquioxane shown in formula II, 5 mol of triethylamine, and 5 mol of xylene solution in a flask, weigh 1.5 mol of acryloyl chloride and add it to a spherical dropping funnel, and place the flask in a water bath Add ice to the water bath, drop acryloyl chloride into the flask at a rate of one drop per second under the ice bath, and stir magnetically; add 1000ppm polymerization inhibitor hydroxyanisole, and stir for 3 hours under the ice bath; after the reaction, Then heat up to 30°C and react for 12 hours; filter the obtained product, then wash with saturated sodium bicarbonate solution for 3 times and separate liquid, water liquid, remove water with anhydrous sodium sulfate, remove solvent by rotary evaporation, and then dry in a vacuum oven at 50°C Drying under the condition for 30 hours, the product containing double bond-modi...
Embodiment 3
[0063] A preparation method containing double bond modified cage silsesquioxane, comprising the following steps:
[0064] Weigh 1 mol of cage-type silsesquioxane shown in formula II, 3 mol of triethylamine, and 5 mol of xylene solution in a flask, weigh 1.5 mol of methacryloyl chloride and add it to a spherical dropping funnel, and place the flask in In the water bath, add ice to the water bath, drop methacryloyl chloride into the flask at a rate of one drop per second under the ice bath, and stir magnetically; add 500ppm of polymerization inhibitor hydroxyanisole, and stir for 2 hours under the ice bath; After the reaction is over, heat up to 25°C for 24 hours; filter the obtained product, then wash with saturated sodium bicarbonate solution for 3 times and separate liquid, water liquid, remove water with anhydrous sodium sulfate, remove solvent by rotary evaporation, and then dry in vacuum Dry in an oven at 40° C. for 24 hours to obtain the double bond-containing modified ca...
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