Polyelectrolyte multilayer films (PEMs) fabricated from the layer-by-layer (LbL) assembly technique have attracted wide interests in the past several decades. Driven and stabilized by electrostatic interaction, the PEMs are sensitive with the external stimuli, contributing to the dynamic tunability of film structures. Compared with adjusting the film structures during assembled procedures, it is more convenient and flexible to control the physical structures of PEMs employing post-treatments. In this review, the different strategies for effectively regulating PEMs’ structures based on the post-treatment, as well as the functionalization of these prepared structural films are discussed. At last, perspectives are provided for the future development directions, aiming to provide opportunities and a novel pathway for microstructural PEMs.
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