Global environmental problems have been increasing with the growth of the world economy and have become a crucial issue.To replace fossil fuels,sustainable and eco-friendly cata-lysts are required for the removal of organic pollutants.In this study,nickel ferrite(NiFe2O4)was prepared using a simple wet-chemical synthesis,followed by calcination;bismuth phosphate(BiPO4)was also prepared using a hydrothermal method.Further,NiFe2O4/BiPO4 nanocomposites were prepared using a hydrothermal technique.Numerous characteri-zation studies,such as structural,morphology,surface area,optical,photoluminescence,and photoelectrochemical investigations,were used to analyze NiFe2O4/BiPO4 nanocompos-ites.The morphology analysis indicated a successful decoration of BiPO4 nanorods on the surface of NiFe2O4 nanoplate.Further,the bandgap of the NiFe2O4/BiPO4 nanocomposites was modified owing to the formation of a heterostructure.The as-prepared NiFe2O4/BiPO4 nanocomposite exhibited promising properties to be used as a novel heterostructure for tetracycline(TC)and Rhodamine B(RhB)removal.The NiFe2O4/BiPO4 nanocomposite de-grades TC(98％)and RhB(99％)pollutants upon solar-light irradiation within 100 and 60 min,respectively.Moreover,the trapping experiments confirmed the Z-scheme ap-proach of the prepared nanocomposites.The efficient separation and transfer of photogen-erated electron-hole pairs rendered by the heterostructure were confirmed by utilizing elec-trochemical impedance spectroscopy,photocurrent experiments,and photoluminescence.Mott-Schottky measurements were used determine the positions of the conduction and va-lence bands of the samples,and the detailed mechanism of photocatalytic degradation of toxic pollutants was projected and discussed.