Spherical bismuth vanadate particles are self-assembled from aqueous Bi(NO3)(3) and NH4VO3 solutions by adjusting pH and tuning the amount of surfactant sodium dodecyl sulfate (SDS) via facile hydrothermal method. The BiVO4 samples were characterized by X-ray diffraction (XRD) and the peaks suited well with the pure phase monoclinic scheelite BiVO4. Field emission scanning electron microscopy (SEM) showed the average size of the spherical particles was 5 mu m and the assembling stages in the hydrothermal synthesis process were recorded. Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) revealed the nanoparticles were single crystal. FT-IR spectroscopy test results demonstrated there was no SDS left in the samples. The mechanism of the self-assembling has also been proposed. (C) 2009 Elsevier B.V. All rights reserved.