Hollow ZnV2O4 spheres with the shell aggregated by small nanoparticles were successfully synthesized through a facile one-pot template-free solvothermal method. The as-prepared product was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), and Brunauer-Emmett-Teller N-2 adsorption-desorption analyses. The formation of ZnV2O4 hollow spheres was based on flowerlike intermediate products supported reduction-dissolution-aggregation process at the expense of consumption of all the flowerlike products. The obtained ZnV2O4 hollow spheres showed a good adsorption capacity of methylene blue (MB) organic dye, which might be attributed to their special structural feature with large surface area. The adsorption kinetics and isotherm of MB on ZnV2O4 hollow spheres were also studied. (C) 2011 Elsevier B.V. All rights reserved.