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In this study, we investigated the influence of TiO2 content and thickness of polystyrene (PS) template on film-formation behavior of PS/TiO2 composites using fluorescence and ultraviolet–visible techniques in conjunction with scanning electron microscopy. Films were prepared by coating PS templates with various layers of TiO2 using dip-coating method. The results showed that PS latexes present complete film formation on top surface of composites. After extraction of PS, a well-defined interconnected porosity were obtained for thin films when TiO2 content was increased, whereas thick samples did not present any interconnected porous structures above a certain TiO2 layer. POLYM. ENG. SCI., 54:288–302, 2014. © 2013 Society of Plastics Engineers