This paper presents new preparation method of Pt/SnO2, an important catalytic system. Besides of its application as a heterogenic industrial catalyst, it is also used as a catalyst in electrochemical processes, especially in fuel cells. Platinum is commonly used as an anode catalyst in low temperature fuel cells, fuelled with alcohols of low molecular weight such as methanol. Platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex was used as a precursor of metallic phase. The aim of the research was to obtain a highly active in electrochemical system Pt/SnO2catalyst with low metal load. Considering small size of Pt crystallites, it should result in high activity of Pt/SnO2system. The presented method of SnO2synthesis allows for obtaining support consisting of nanoparticles. The effect of the thermal treatment on activity of Pt/SnO2gel was demonstrated. The system properties were investigated using TEM, FTIR (ATR), and XRD techniques to describe its thermal structural evolution. The results showed two electrocatalytical activity peaks for drying at a temperature of 430 K and above 650 K.