Titanium Di-oxide (TiO2) powder samples mixed with Polyethylene Glycol (PEG) were synthesized using sol-gel processing followed by solvent evaporation. Temperature induced crystallization, PEG removal and phase transition were studied using differential thermal analysis (DTA) in combination with Thermo gravimetric (TG) analysis. Crystallization with brookite structure followed by PEG decomposition was recorded below 324 degrees C resulting a three-dimensional (3D) as well as,mesoporous TiO2. BET surface area measurements revealed that the pore size was evolved between 332 nm and 12.54 nm depending upon the calcinations temperature. It is observed that the phase transition from brookite to anatase phase was resulting in crashing of porosity. (C) 2016 Elsevier B.V. All rights reserved.