In this work, we prepared TiO2 and Co multilayer thin films via DC magnetron sputtering method on (100) GaAs and (100) Si substrates. The power for each target (TiO2 and Co), deposition time of the layers, and pressure during deposition were kept constant. From XRD, Raman, and IR measurements, the formation of the rutile and triclinic Co phases were identified in the multilayer thin films. An annealing process was carried in situ on all samples and subsequent to the deposition stage during 2 h. The substrate used was GaAs and Si wafer, favoring the formation and growth of the found phases. The diffusion and interdiffusion of the layers in the thin films were determined from Rutherford Backscattering Spectroscopy (RBS). In particular, Co and Ga were observed to associate after the annealing process according to the depth profiles. Due to the interdiffusion layers, the parallel magnetic contribution is not significant in the bilayer. Curves I-V of the Co/TiO2 bilayer showed the presence of resistive switching, according to the bipolar resistive. A correlation between synthesis parameters and the physical properties of the multilayers is presented. © 2020 Elsevier Inc.