Mixed tin-iridium oxide (Sn 0.85 Ir 0.15 O 2 ) nanoparticles at low Ir content (15 mol%) were prepared by the sol-gel preparative route, varying calcination temperatures in the range 450-550°C. The crystal structures, the phase composition and crystallite sizes were analyzed by X-ray powder diffraction (XRD). The local order of the materials was investigated by Raman spectroscopy. X-ray photoelectron spectroscopy (XPS) analysis revealed the variation of the Ir surface state with the temperature of firing. The morphology of crystallites and the aggregates were analyzed by high resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM), respectively. Nitrogen physisorption by BET method was adopted to evaluate the particle surface area and the mesopore volume distribution. Electrochemical properties of the Ti-supported powders were evaluated by cyclic voltammetry (CV) and quasi steady-state voltammetry.