Nano-crystalline CeO2 was synthesized by the mechanical milling and subsequent heat-treatment from the mixture of Ce(OH)4 as precursor, and NaCl as diluent. The diluent provided diffusion barrier during milling and heat-treatment, which was easily dissolved out by deionized water. The size of crystallite and the strain variance of CeO2 were depended on the temperature and heat-treatment time: increased with the temperature (400~700oC) and time (1~24 hours) increasing, and saturated near at 20nm in size owing to the densification of diluent. The synthesized nano-crystalline CeO2 powder was applied as an abrasive in CMP (Chemical Mechanical Planarization) slurry. When blanket-type SiO2 and Si3N4 wafers were polished with the slurries, the removal rates (RR) of SiO2 and Si3N4 wafers and selectivities (RRSiO2/RRSi3N4) were influenced by synthetic condition of abrasive, the suspension stability and the pHs of slurries.