A single‐step sonochemical procedure to synthesize hybrid vanadium oxide/polyaniline nanowires starting from crystalline V2O5 and aniline in aqueous medium is presented. The synthesis explores the effect of high power ultrasounds on heterogeneous solid–aqueous phases, which leads to 30 nm width wires of 5 to 10 µm in length. Monomer intercalation and oxidative polymerization within the inorganic matrix proceed simultaneously with morphological changes. The electronic conductivity of hybrid nanowires reaches 0.8 S · cm−1 at room temperature.
