Organic-inorganic composite microspheres with PS as a core and CeO2 nanoparticles as a shell were synthesized by in situ decomposition reaction of Ce(NO3)(3) on the surfaces of PS microspheres prepared through soap-free emulsion polymerization. The shell thickness of the composite microspheres could be turned by varying the concentration of Ce(NO3)(3) in the reaction solution. The whole process required neither surface treatment for PS microspheres nor additional surfactant or stabilizer. The as-synthesized PS/CeO2 composite microsphere samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). Oxide chemical mechanical polishing (CMP) performance of the PS/CeO2 composite abrasives with different shell thickness was characterized by atomic force microscopy (AFM). The results indicated that the as-prepared core-shell structured composite microspheres (220-260 nm in diameter) possessed thin shell (10-30 nm) composed of CeO2 nanoparticles (particle diameter of 5-10 nm), and the final CeO2 contents of the composite microspheres ranged from 10 to 50 wt%. A possible mechanism for the formation of PS/CeO2 composite microspheres was discussed also. The CMP test results confirmed that the novel core-shell structured composite abrasives are useful to improve oxide CMP performance. In addition, there is an obvious effect of shell thickness of the composite abrasives on oxide CMP performance. (C) 2011 Elsevier B.V. All rights reserved.