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An intrinsic dilemma exists for block copolymer vesiclesimproving the colloidal stability of vesicles using long/charged stabilizing blocks lowers the propensity of morphological transition to vesicles. Moreover, maintaining the vesicular morphology requires effective structure stabilization via cross-linking. We report a strategy to circumvent this problem and simultaneously improve the colloidal and structural stability of vesicles synthesized via polymerization-induced self-assembly (PISA) using dispersion polymerization. More specifically, in situ cross-linked poly­(N,N-dimethyl­acrylamide)-b-poly­(diacetone acrylamide-co-allylacrylamide) diblock copolymer vesicles are first synthesized via aqueous dispersion polymerization, which then serve as a robust platform to initiate the growth of a third hydrophilic block of either neutral poly­(N,N-dimethyl­acrylamide), anionic poly­(2-acrylamido-2-methyl-1-propane­sulfonic acid sodium salt), or cationic poly­(3-acrylamido­propyl trimethyl­ammonium chloride) with retained vesicular morphology. The formed cross-linked triblock copolymer vesicles have advantages of diverse surface chemistry and arbitrary stabilizing block length. As a control experiment, synthesis from linear diblock copolymer vesicles provides a mixture of triblock copolymer vesicles and spheres. The successful synthesis of triblock copolymer vesicles with a binary mixture of two hydrophilic stabilizing blocks is supported by dynamic light scattering (DLS), transmission electron microscopy (TEM), electrophoresis, and X-ray photoelectron spectroscopy (XPS). Both linear and cross-linked triblock copolymer vesicles are subjected to solvent dissolution, freeze-drying, and surfactant challenge studies, which collectively demonstrate that cross-linked triblock copolymers can maintain their vesicular structure and show excellent colloidal and structural stability, as indicated by DLS, TEM, and transmittance measurements.

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