This paper deals with a simple FTO/p-n heterojunction electrode assembly formed by BiVO 4 and NiO thin films, where the precursor solution is obtained by solution combustion synthesis and precipitation in aqueous media techniques, respectively, whereas the thin films were deposited by the dip-coating deposition process. The FTO/p-n electrodes are characterized by X-ray diffraction, scanning electron microscopy, Raman spectroscopy and UV-Vis spectroscopy. The performance analysis based on the methylene blue degradation reaction have shown that the p-n electrodes, FTO/p-NiO/n-BiVO 4 and FTO/n-BiVO 4 /p-NiO have higher electroactivity under visible light irradiation condition when compared to single BiVO 4 thin film, deposited separately, with estimated k obs value of 340 9 10-4 min-1 , 270 9 10-4 min-1 and 150 9 10-4 min-1 , respectively.