In this study, we have studied the effect of repeated annealing temperatures on TiO2 thin films prepared by dip-coating sol-gel method onto the glasses and silicon substrates. The TiO2 thin films coated samples were repeatedly annealed in the air at temperatures 100, 200, and 300 A degrees C for 5 min period. The dipping processes were repeated 5 to 10 times in order to increase the thickness of the films and then the TiO2 thin films were annealed at a fixed temperature of 500 A degrees C for 1 h period. The effect of repeated annealing temperature on the TiO2 thin films prepared on glass substrate were investigated by means of UV-VIS spectroscopy, X-ray diffraction (XRD), and atomic force microscopy (AFM). It was observed that the thickness, average crystallite size, and average grain size of TiO2 samples decreased with increasing pre-heating temperature. On the other hand, thickness, average crystallite size, and average grain size of TiO2 films were increased with increasing number of the layer. Al/TiO2/p-Si metal-insulator-semiconductor (MIS) structures were obtained from the films prepared on p-type single silicon wafer substrate. Capacitance-voltage (C-V) and conductance-voltage (G/omega-V) measurements of the prepared MIS structures were conducted at room temperature. Series resistance (R (s)) and oxide capacitance (C (ox)) of each structures were determined by means of the C-V curves.