Potassium-substituted SrFeO3-δ for possible application as oxygen evolution electrode in alkaline or molten salt media was prepared by mechanical activation and characterized by X-ray diffraction, dilatometric and thermogravimetric analysis, Mössbauer spectroscopy, and electrical conductivity measurements. Room temperature mechanical activation of a mixture of oxide precursors with subsequent thermal treatments at 700-900 °C results in the formation of Sr0.9K0.1FeO3-δ with tetragonal perovskite-like structure. Such allows to decrease the synthesis temperature, if compared to the conventional solid-state route, and to prevent possible volatilization of potassium. The results of Mössbauer spectroscopy studies indicate that the oxygen nonstoichiometry in the samples annealed in air at 900-1100 °C with subsequent rapid cooling vary in the range δ=0.30-0.32. The electrical conductivity in air exhibits a metal-like behaviour at temperatures above 400 °C and semiconductor behaviour in the low-temperature range, reaching 13-30 S/cm under prospective operation conditions for alkaline electrolyzers (≤90 °C). © 2012 Elsevier Inc.