The b-Ni(OH) 2 microspheres have been fabricated by a facile hydrothermal method in the assistance of biomolecule (L-arginine). The NiO microspheres were obtained with further calcination of b-Ni(OH) 2 precursor at 500°C for 2 h. Subsequently, Ag/NiO nanocomposite microspheres were also prepared by the reduction of AgNO 3 solution. The as-synthesized products were characterized by X-ray power diffraction, scanning electron microscopy, transmission electron microscopy, energydispersive X-ray spectroscopy, thermogravimetric analysis et al. The photocatalytic activity of Ag/NiO composite microspheres was also investigated by UV-Vis spectrophotometer and the results display enhanced photocatalytic activity in degradation of methyl orange.