This paper reports the synthesis of nanosized Ag/Co3O4 composite catalysts using a silver-mirror reaction and the calibration of their catalytic activities towards methyl blue (MB) dye degradation with peroxymonosulfate (PMS) under visible light. The nanosized Ag/Co3O4 composites were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV-vis spectroscopy. The experimental evidence indicated that the hydrothermal synthesis approach lead to the exposure of the {1 1 2} facets of the Co3O4 nanoflakes. Compared to Co3O4 nanoflakes, Co3O4 doped with Ag nanoparticle (average diameters of 10-15 nm) presented lower band gap energy and photoluminescent (PL) intensity. Meanwhile, the Ag/Co3O4 exhibited high stability and excellent dispersion property in dye solution. Experimental data suggested that 3.06 wt% Ag nanoparticle-doped Ag/Co3O4 nanocomposite catalyst possessed the highest catalytic activity towards MB degradation in aqueous solution at the tested concentration level of 15 mg/L, about 2.4 times higher than that of pure Co3O4. Complete decolorization of the 15 mg/L MB solution can be achieved by 3.06 wt% Ag-doped Ag/Co3O4 nanocomposite within 20 min of visible light irradiation. (C) 2015 Elsevier B.V. All rights reserved.