Vanadium oxide catalyst supported on TiO2-ZrO2 has been prepared by adding Ti(OH)4-Zr(OH)4 powder to an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The char-acterization ofthe prepared catalysts was performed using solid-state 51V NMR and FTIR.In thecase ofcalci-nation temperature at 773 K, vanadium oxide was in a highly dispersed state for the samples containing low loading V2O5 below 25 wt %, but for samplescontaining high loading V2O5 equal to or above 25 wt %, vana-dium oxidewas well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2.The ZrV2O7 compound was formed through the reactionof V2O5 and ZrO2 at 773-973 K, where-as the V3Ti6O17 compound was formedthrough the reaction of V2O5 and TiO2 at 973-1073 K. The V3Ti6O17 compound decomposed to V2O5 and TiO2 at 1173 K, which were confirmed by FTIR and 51V NMR.