In this study, polythiophene-TiO 2 nanotube films (PTh/TNT) were successfully prepared by a two-step electrochemical process of anodizaton and electropolymerization, in which a highly-ordered TiO 2 nanotube (TNT) film was anodized at a low-voltage with post calcination first and then the prepared TNT film was deposited with a polythiophene layer by electropolymerization in the BFEE electrolyte. The morphology and structures of PTh/TNT composites were examined by FESEM, EDX, XRD, and XPS methods. XPS spectra of PTh/TNT composites indicate the strong interaction between S sites of polymer backbone and TiO 2 nanotubes, in which electron transfer from polythiophene to titania takes place. UV-vis DRS analysis shows that these composites have a strong photoresponse in the visible region at 500 nm. The prepared PTh/TNT films revealed significant activity for 2,3-DCP degradation under visible light irradiation and also sunlight irradiation, in which the PTh3/TNT film achieved the best performance. On the other hand, this study also confirmed that the sidechains of polythiophene could influence its photocatalytic activity significantly in an order from high to low as poly3-methylthiophene ≈ polythiophene > polythiophenecarboxylic acid > poly3-hexylthiophene. The results may provide useful information to further develop This is the Pre-Published Version.2 some effective polymer-semiconductor catalysts for pollutant degradation under sunlight irradiation for water and wastewater treatment.