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Nanometer cerium-zirconium oxide solution Ce1-x ZrxO2 was synthesized by mechanically activated solid state re-action at middle-low temperatures, with Ce2(CO3)3, ZrOC12-8H2O and H2C2O4.2H2O as raw materials. The crystal structureand microstructure of the nanometer Ce1-xZrxO2 were studied with X-ray diffractometry (XRD) and transmission electronmicroscope (TEM). The results show that the product is single-cubic-phase solid solution with an average crystal size 19.64nm. In this article, the influence of surface active agent is also evaluated. Mechanically activated solid state reaction for thepreparation of Ce1-xZrxO2 is a new technique of green chemistry without solvent and waste.