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This article reports the synthesis and photoinduced mass-migration behavior of two amphiphilic side-chain azo diblock copolymers (PEG-b-P2CN, PEG-b-P6CN), which contain ethylene and hexamethylene as flexible spacers between main chains and pendent azobenzene functional groups. The copolymers were synthesized by atom transfer radical polymerization (ATRP) to obtain precursor block copolymers from a PEG-based macromolecular initiator and postpolymerization azo-coupling reaction of the precursors to introduce the azo chromophores. Spectroscopic analyses, GPC, and thermal analyses indicated that the diblock copolymers possessed well-defined structures and narrow molecular weight distributions. The photoinduced mass-migration behavior was studied through two different approaches, that is, investigating photoinduced deformation of colloidal spheres of the copolymers and surface relief …