A series of poly(vinylphenol-b-vinylpyridine) (PVPh-b-P4VP) block copolymers were prepared through anionic polymerizations of 4-tert-butoxystyrene with 4-vinylpyridine followed by subsequent selective hydrolysis of the 4-tert-butoxystyrene protective groups. Infrared spectrum analysis suggests that this block copolymer possesses strong hydrogen-bonding interaction between the hydroxyl group of PVPh and the pyridine group of P4VP. DSC analyses indicate that these PVPh-b-P4VP copolymers always have higher glass transition temperatures than the corresponding PVPh/P4VP miscible blends obtained from DMF solution. However, the thermal behavior of PVPh-b-P4VP diblock copolymer shows a similar T g value with the PVPh/P4VP blend complex obtained from methanol solution at a 1:1 (PVPh:P4VP) molar ratio. We proposed that the polymer chain behavior of the PVPh/P4VP blend from DMF solution is separated coils. However, by increasing the hydrogen bonding for PVPh-b-P4VP diblock copolymer, a polymer complex aggregate is proposed, which is similar to the PVPh/P4VP blend complex from methanol solution. The spin−lattice relaxation time in the rotating frame ( ) based on solid-state NMR analysis is able to provide positive evidence that the polymer complex aggregate in the diblock copolymer has a shorter value than the separated coils in the miscible blend.

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Poly(vinyl phenol)‐block‐polystyrene (PVPh‐b‐PS) diblock copolymers are synthesized by sequential anionic polymerization with sec‐butyl lithium as the initiator. The PVPh‐b‐PS diblock copolymer is cast (on a substrate) from several solvent mixtures that contain tetrahydrofuran/toluene ratios of 1:0.1, 1:1, and 1:2. After solvent evaporation the resulting films are characterized by SEM, TEM, and contact angle measurements. A honeycomb structure is fabricated from the vesicle structure at relatively low toluene contents. On the contrary, at relatively higher toluene contents, a micelle structure with porous microspheres is formed, which possesses higher surface roughness and results in film surface superhydrophobicity. The simple method described here that uses common/selective mixed solvents may be easily extended to prepare honeycomb structures and superhydrophobic surfaces simultaneously from a wide variety of block copolymers by carefully controlling the weight composition of the block copolymer and the selective solvent content.

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