The semiconductor's realization is a very significant stage of optoelectronics devices. In this work, an elaboration of the TiO2 semiconductor is made with various solution flow rates via spray pyrolysis. The structural and optical properties of pure TiO2 are investigated with several characterization techniques which include: X‐ray diffraction (XRD), Raman spectroscopy, and UV–vis spectrophotometry. The XRD of elaborated TiO2 layers exhibits nanocrystalline nature with a preferential orientation at the (101), a unique phase of anatase TiO2. The apparition of vibration modes in Raman spectra confirms the TiO2 formation with a single phase. The produced TiO2 has an optical transmission varying from 90% to 70% in the visible wavelength. The energy band gaps are 3.42, 3.32, and 3.28 eV for the TiO2 elaborated at 1, 1.5, and 2 mL min−1, respectively which prove the semiconducting properties of TiO2. All other optical parameters such as refractive index (n), extinction coefficient (k), and dielectric constant (εr, εi) vary with the variation of solution flow rate. These investigations discover that the properties of TiO2 layers can be adjusted by solution flow rate. It seems that the process of spray pyrolysis provides a facile way to control the quality of TiO2 thin layers.