Microphase Separation within Disk Shaped Aggregates of Triblock Bottlebrushes

Well‐defined AbBA 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 bB block is prepared by controlled radical polymerization and click chemistry. The triblock copolymer with a composition of PAm₂₀₀‐b‐b(PBA₁₄‐b‐PS₄₇)₁₆₇‐b‐PAm₂₀₀ is obtained and is further transformed into PAm₂₀₀‐b‐b(PAA₁₄‐b‐PS₄₇)₁₆₇‐b‐PAm₂₀₀ 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 bB block, PAm₂₀₀‐b‐b(PAA₁₄‐b‐PS₄₇)₁₆₇‐b‐PAm₂₀₀ 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.