As an effective photocatalyst, PANI/NiFe2O4 nanocomposite was prepared by in situ polymerization of aniline. The physicochemical properties of the composite were characterized by TEM, XRD, FT-IR spectra, UV-vis spectroscopy, XPS and Photoelectrochemical Measurements. Compared with NiFe2O4 and PANI, PANI/NiFe2O4 nanocomposite has a better photocatalytic activity, which exhibited the remarkable property of hydrogen production under visible light. The photocatalytic mechanism was also discussed. The heterojunction of PANI and NiFe2O4 promoted the separation of photogenerated e(-) and h(+) on the surface of PANI/NiFe2O4. Besides, the structure of PANI/NiFe2O4 in the polymerization was detected by FT-IR. NiFe2O4 was proved that in favor of the formation of nucleate phenazine-like structure in the progress of in situ polymerization. Then the chain structure of conductive PANT was formed, which leading to the promotion of photocatalytic activity. (C) 2017 Published by Elsevier Ltd on behalf of Hydrogen Energy Publications LLC.