Cobalt oxide and composite thin films were synthesized by spin-coating technique, followed by heating to 500°C in oxidizing, inert, or reducing atmospheres. Methanolic solutions of triethanolamine complexes of cobalt acetates and nitrates were spin-coated at 1000, 2000, and 3000 rpm. The influence of heating parameters and film thickness on the phase content of the films were investigated, using grazing incidence X-ray diffraction, X-ray reflectivity, and scanning electron microscopy. By tuning the synthesis parameters, Co 3 O 4 , CoO and Co films were obtained, as well as CoO-Co and Co 3 O 4 -CoO composite films of varying phase ratios.