BiSbO(4) nanoplates with a large BET specific area has been prepared successfully via a facile hydrothermal reaction from Sb(2)O(3) and Bi(NO(3))(3). The effects of reaction conditions and the precursors on the final products were investigated. It is proposed that the redox reaction between Sb(2)O(3) and Bi(NO(3))(3) plays a pivotal role in the formation of nanocrystalline BiSbO(4). The hydrothermally prepared nanocrystalline BiSbO(4) was characterized by X-ray diffraction (XRD), N(2)-sorption BET surface area, UV-vis diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The DRS result clarifies that BiSbO(4), originally believed to be a visible light responsive photocatalyst, is indeed UV light responsive with a band gap of 3.5 eV. The existence of Bi containing an impurity may be responsible for the visible light response of BiSbO(4) prepared via a conventional solid state reaction. BiSbO(4) nanoplates prepared via the hydrothermal method showed superior photocatalytic performance for the degradation of benzene and 4-chlorophenol (4-CP) as compared to BiSbO(4) prepared via a solid state reaction and Degussa P25. BiSbO(4(Hy)) nanoplates can be a promising photocatalyst in the treatment of environmental pollution.