Nanocrystalline titania powder was prepared at room temperature via sol-gel method; using TiCl4 as precursor and absolute ethanol solution. After mixing, the gel solution was formed. Then the sol-gel dried and calcined at different temperatures. The size of the prepared nanoparticles was reduced by Nd-YAG Pulse Laser Ablation (PLA). The characterization of the TiO2 Nanoparticles in two phases was carried out by X-ray Diffraction (XRD) to investigate the phase structure. The Transmission Electron Microscope (TEM) result shows the particle size of nanoparticles after laser ablation less than 10 nm. Scanning Electron Microscopy (SEM) to obtain the surface morphological studies Results showed that anatase was the only phase in titanium oxide powders up to 500 °C, when the calcination increased in the region of 900 °C the phase transformation from anatase to rutile occurred in the TiO2 nanopowders. This paper shows a comparison between two phases of TiO2 Nanoparticles (anatase and rutile). Fourier Transform Infra-Red (FTIR) to study the vibrational frequencies between the bonds of atoms for synthesized TiO2 Nanoparticles. The Crystalline size of TiO2 Nanoparticles obtained was between (15 -70) nm for anatase at 500 °C and rutile at 900 °C. In FTIR analysis, all the peaks observed were around (400-700) cm-1 due to stretching and bending vibrations.