The paper details with of the preparation and physicochemical characterisation of nano- and microstructured TiO₂ doped with Fe and Co produced by the sol-gel method using titanium alkoxide as the precursor of titania as well as iron or cobalt nitrates as dopant sources. Fe and Co doped TiO₂ materials were successfully prepared with two different methods. The effect of the dopant type on the synthesis of TiO2 powders was investigated. The physicochemical properties of the studied samples were determined. The characterisation included determination of the dispersion and morphology of the systems (particle size distribution, SEM images), characteristics of porous structure (BET isotherms), crystalline structure (XRD), surface composition (EDS), as well as thermal stability (TG/DTA).