摘要： Graphitic carbon nitride (g-C3N4) based catalysts are evolving in energy harvesting applications due to their robustness, nontoxicity, and most important photocatalytic efficiencies. In this work, we successfully engineered g-C3N4/Nb2O5 type (II) heterojunction via pulse sonochemical technique based on opposite charge-induced hetero-aggregation on the surface. The agglomerated spherical Nb2O5 nanoparticles (NPs) having diameter 30-40 nm observed on the lamellar surface of g-C3N4 in FESEM images. The XRD and XPS analysis confirm the orthorhombic phase and formation of the g-C3N4/Nb2O5 heterostructure. The FTIR spectra of g-C3N4/Nb2O5 show characteristic poly s-triazine bands from 1250 to 1650 cm-1. Moreover, g-C3N4/Nb2O5 exhibited the lower bandgap value of 2.82 eV as compared to Nb2O5 (3.25eV) with significant redshift and enhance visible light absorption. The Mott-Schottky (MS) analysis confirms the formation of heterojunction between g-C3N4 and Nb2O5, with significant band shifting towards lower hydrogen evolution reaction (HER) potential. The g-C3N4/Nb2O5 heterojunctions showed many folds enhanced photocurrent response from photoelectrochemical (PEC) water splitting, and the value reached to – 0.17 mA/cm2 with good stability and insignificant dark photocurrent at 1.0 V vs RHE. The electrochemical impedance spectroscopic (EIS) measurements further elucidate the suppression of photogenerated electrons/holes as the radius of the semicircle significantly decreased in case of heterojunction formation. The enhanced photocatalytic hydrogen generation by the heterostructures could be attributed to the effective formation of heterojunctions between the g-C3N4 and Nb2O5 semiconductors, causing the migration of the photogenerated electrons and holes, hence increasing their lifetimes.