ABSTRACT. In this study, the CaCO3 powder has successfully been synthesized by mixing CaCl2 derived from natural limestone and Na2CO3 in the same molar ratio. The mixing process of two solutions was performed by employing the molar contents of 0.25, 0.5, 0.75 and 1 M at varying temperatures of 35, 50 and 80ᴼC. The produced CaCO3 microparticles were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Brunauer-Emmett-Teller (BET). The highest content of vaterite phase of the samples is around 96 wt%, resulted from the process using solution of 0.25 M at 35ᴼC. All the samples prepared show mesoporous solids with pore sizes of 3-4 nm and specific surface area of 81-90 m 2 /g.