K4Nb6O17 nano-layered compound was obtained by solid-phase synthesis and then methylene blue (MB) was intercalated into layered niobate K4Nb6O17 interlayer I by a two-step guest-guest exchange method using the intercalation compound, methyl viologen (MV2+)-K4Nb6O17, as precursor. The optically transparent MB+-K4Nb6O17 nanocomposite thin film has been characterized by XRD, IR, TGA, elemental analysis, UV, and electrochemical measurements. It was estimated that the intercalated MB+ ions are mainly aggregated. The cyclic voltammogram of the MB+-K4Nb6O17 nanocomposite thin film exhibited a fine diffusion-controlled cathodic process, which hints the possibility of being utilized as an electrode modifying material.