In the present work iron oxide nanoparticles have been synthesized by alkaline solvo thermal method using anhydrous ferric chloride, sodium hydroxide, polyethylene glycol and cetyl trimethyl ammo nium bromide and characterized by X ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Field Emission Scanning Electron Microscopy (FESEM), Energy dispersive X ray Spectroscopy (EDX) and Thermal Gravimetric Analysis (TGA). XRD indicated that the product is a mixture of different phases of iron oxide viz. gamma Fe 2 O 3 (maghemite, tetragonal), Fe 2 O 3 (maghemite, cubic), Fe 3 O 4 (magne tite, cubic) and ε Fe 2 O 3 (epsilon iron oxide). FESEM studies indicated that size of the particles is observed in the range of about 19.8 nm to 48 nm. EDX spectral analysis reveals the presence of carbon, oxygen, iron in the synthesized nanoparticles. The FTIR spectra indicated absorption bands due to O-H stretching, C-O bending, N-H stretching and bending, C-H stretching and Fe-O stretching vibrations. TGA curve repre sented weight loss of around 3.0446 % in the sample at temperature of about 180°C due to the elimination of the water molecules absorbed by the nanoparticles from the atmosphere.