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 heteroaggregation 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 (3.25 eV) 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 toward 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.