Abstract: The samples of Na0.7CoO2 polycrystals have been synthesized by solid-state reaction according to corresponding components chemical molar ratio.The result of XRD measurements has demonstrated shown that the Na0.7CoO2 samples are of the single-phase polycrystals.Under the temperature the mixture of ice and water,the Raman spectrum of measurements has also proved that the Na0.7CoO2 polycrystals have the characteristic with accurate composition and single phase.The high drive energy and big specific surface areas of the Co3O4 particles with average dimension is at 20-50nm are the major factors that the preparation for (Na0.7CoO2) in our case does not demand oxygen atmosphere gas and has lower sintering temperature than which in literature 1.