Uniformly-shaped, spherical RuO2/TiO2 particles were synthesized exclusively by one-step ultrasonic spray pyrolysis USP) of a mixture of n-butylorthotitanate and ruthenium chloride acidic aqueous solutions. The USP temperature was 200 degrees C -quite below the typical conversion temperatures of the precursors to the oxides. Basic electrochemical properties of RuO2/TiO2 USP powders as-prepared or additionally dried and/or thermally treated) in the form of a thin layer applied onto glassy carbon electrode are investigated and compared to the properties of powder synthesized at quite higher temperature of 800 degrees C. The coatings of activated titanium anode ATA) were prepared from RuO2/TiO2 USP powders in order to check the anode electrolysis stability and to correlate the anode properties to those of native USP powders. Low-temperature material showed much better performances than high-temperature one. ATA obtained from low-temperature USP powder showed considerably higher stability. The obtained results are found to be in close correlation to the powder and coating structure, composition and morphology affected by subsequent thermal treatment of the material synthesized at low USP temperature.