Herein, for the first time, a direct Z-scheme g-C 3 N 4 /NiFe 2 O 4 nanocomposite photocatalyst was prepared using facile one-pot hydrothermal method and characterized using XRD, FT-IR, DRS, PL, SEM, EDS, TEM, HRTEM, XPS, BET and VSM characterized techniques. The result reveals that the NiFe 2 O 4 nanoparticles are loaded on the g-C 3 N 4 sheets successfully. The photocatalytic activities of the as-prepared photocatalysts were evaluated for the degradation of methyl orange (MO) under visible light irradiation. It was shown that the photocatalytic activity of the g-C 3 N 4 /NiFe 2 O 4 nanocomposite is about 4.4 and 3 times higher than those of the pristine NiFe 2 O 4 and g-C 3 N 4 respectively. The enhanced photocatalytic activity could be ascribed to the formation of g-C 3 N 4 /NiFe 2 O 4 direct Z-scheme photocatalyst, which results in efficient space separation of photogenerated charge carriers. More importantly, the as-prepared Z-scheme photocatalyst can be recoverable easily from the solution by an external magnetic field and it shows almost the same activity for three consecutive cycles. Considering the simplicity of preparation method, this work will provide new insights into the design of high-performance magnetic Z-scheme photocatalysts for organic contaminate removal.