Some zirconia-supported vanadium oxides have been prepared by set-gel method and characterized by different techniques. The vanadium content exerts an effect on the a rea and pore-size of precursors and samples calcined. The presence of vanadium also affects the decomposition of precursors into ZrO2 and to its phase transformation, as well as the formation of fibres, as shown by SEM-EDX. XPS analyses show the presence of two species of vanadium at the surface, V5+ and V4+, the percentage of each one depending on the load of vanadium in the catalyst.