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Amphiphilic diblock copolymers may assemble in aqueous solutions to form vesicles delimited by a polymeric double layer, also known as polymersomes, considered a more robust option to liposomes. Diblock copolymers may respond to pH, temperature, and other conditions. Because of such properties, polymersomes are currently being studied as drug delivery systems or as nanoreactors. pH-responsive polymersomes are potentially crucial because unusual pH gradients are present in cells under several physiological and pathological conditions. We synthesized two diblock copolymers of poly [2-(dimethylamino) ethyl methacrylate]-block-polystyrene (PDMAEMA-b-PS) via RAFT. We both developed new materials and better-understood polymersomes' properties with pH and temperature-responsive groups with these polymers. GPC, 1H-NMR, and FTIR characterized copolymers. The ionization equilibrium of the PDMAEMA amino groups on the polymersomes was analyzed by potentiometric titration and Zeta potential measurements. The hydrodynamic radius of the polymersomes in different pH and temperatures was analyzed by DLS. Entrapment of an electron paramagnetic resonance probe indicated the presence of a hydrophilic inner core. Negative staining transmission electron microscopy showed spherical aggregates and confirmed the diameter around 80 nm. These polymersomes with dual stimulus–response (i.e., pH and temperature) may be a platform for gene delivery and nanoreactors. [ABSTRACT FROM AUTHOR]