Microphase Separation within Disk Shaped Aggregates of Triblock Bottlebrushes

Well‐defined A b BA triblock bottlebrush with poly(N,N‐dimethyl acrylamide) (PAm) as A block and polyacrylate, densely grafted with poly( tert ‐butyl acrylate)‐ block ‐polystyrene (PBA‐ b ‐PS), as brush b B block is prepared by controlled radical polymerization and click chemistry. The triblock copolymer with a composition of PAm 200 ‐ b ‐ b (PBA 14 ‐ b ‐PS 47 ) 167 ‐ b ‐PAm 200 is obtained and is further transformed into PAm 200 ‐ b ‐ b (PAA 14 ‐ b ‐PS 47 ) 167 ‐ b ‐PAm 200 by hydrolysis of the PBA segment into poly(acrylic acid) (PAA). In a mixture of N,N‐dimethylformamide (DMF) and methanol, a poor solvent of b B block, PAm 200 ‐ b ‐ b (PAA 14 ‐ b ‐PS 47 ) 167 ‐ b ‐PAm 200 self‐assembled into disk‐like platelets, which have an internal lamellar structure by further microphase‐separation of PAA‐ b ‐PS branches in 2D. Moreover, Ag nanoparticles are aligned by PAA segments along the disk to form a pattern.