This study evaluated the effect of crystallization temperature (300, 500 and 700 °C) on the photocatalytic and photoluminescent properties of the multilayer thin films of TiO 2 , In 2 O 3 and TiO 2 /In 2 O 3 which were prepared by the Complex Polymerization Method (CPM) and deposited on substrates of Si (100) by the spin coating method. The results of X-ray diffraction (XRD) revealed that there was no chemical interaction between the oxides (TiO 2 /In 2 O 3 ) in crystalline films. The morphology was observed by atomic force microscopy (AFM) with a mean grain size of 15-35 nm. The result showed that the photocatalytic property is significantly increased by increasing the crystallization temperature. This is due to the agitation of the molecules which facilitates the transfer of charge between the electron and the catalyst bore. UV-vis light absorption spectra indicated that the addition of In 2 O 3 in TiO 2 films is an effective way of increasing the uptake of TiO 2 in the visible region up to ~ 600 nm for photocatalytic applications, it was also possible to observe that these films could be easily Recycled for reuse. The samples were also characterized by photoluminescence, where it was possible to observe that the reduction of the PL intensity increased the photocatalytic activity of the thin films, with the increase of the crystallization temperature. In addition, the method used in this study is simple and economical compared to other methods.