In the present study, Titanium Dioxide (TiO2) was prepared by microwave assisted sol-gel synthetic method and effect of heat treatment on microcrystalline properties was studied. Synthesized material was sintered at three different temperature; 400, 500 and 600 °C. To investigate microstructural properties, samples were introduced to X-Ray diffraction (XRD), scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS) UV-Visible spectroscopy. XRD pattern depicts semicrystalline behaviour of unannealed TiO2 which was converted into perfect crystalline nature at higher thermal treatment. Exhaustive growth of tetragonal anatase phase of TiO2 was observed. However, the TiO2 annealed at 600 °C traces of rutile phase was also observed which reflects phase transformation at higher annealing temperature. The absorption spectra shows that all the samples are UV active as they absorb UV radiation strongly. FE-SEM images shows clusters of spherical particles in the range of 20-30 nm..