The present work describes the results of investigation of structure TiO2 depending on temperature and thermal treatment conditions. The structural characteristics of the samples were evaluated using X-ray diffraction, SEM and Raman spectroscopy. Cylindrical-shaped TiO2 ceramic specimens were prepared from plastic TiO2 ceramic mass by extrusion. Plastic ceramic mass was obtained by mixing the required components (TiO2 (anatase) powder, distilled H2O, binder and oil). Dried samples were sintered in air followed by thermal treatment in high vacuum conditions (2×10-3 Pa). XRD patterns of all samples treated in vacuum, showed the presence of rutile crystalline structure. To compare morphology of the raw materials and obtained samples SEM was used. Raman spectra were measured using Renishaw inVia micro-Raman spectrometer equipped with argon laser (514.5 nm, max cw power Pex=10 mW). The spectral signal was dispersed by the 2400 grooves/mm grating onto Peltier-cooled (-60C) CCD detector.