Summary: The bis‐hydrophilic block copolymer, poly(acrylic acid)45‐block‐poly(N,N‐diethylacrylamide)360, was obtained after hydrolysis of poly(tert‐butyl acrylate)45‐block‐poly(N,N‐diethylacrylamide)360, synthesized by sequential anionic polymerization of tert‐butyl acrylate (tBA) and N,N‐diethylacrylamide (DEAAm) in the presence of Et3Al. The polymer is stimuli‐sensitive with respect to both pH and temperature in aqueous solution, reversibly forming spherical crew‐cut micelles with PDEAAm‐core (〈Rh〉z = 21.5 nm) under alkaline conditions for T > 35 °C as well as inverse star‐like micelles with an expanded PAA‐core (〈Rh〉z = 43.8 nm) under acidic conditions for T < 35 °C, as indicated by dynamic light scattering.
Modes of micelle formation for poly(acrylic acid)45‐block‐poly(N,N‐diethylacrylamide)360 in aqueous solution depending on the pH and temperature.