In this study, an aerosol process was introduced to produce CaCO3. The possibility of producing CaCO3 by the aerosol process was evaluated. The characteristics of CaCO3 prepared by the aerosol process were also evaluated. In the CaCO3 prepared in this study, as the heat treatment proceeded, the calcite phase disappeared. The portlandite phase and the lime phase were formed by the heat treatment. Even if the CO2 component is removed from the calcite phase, there is a possibility that the converted CO2 component could be adsorbed into the Ca component to form a calcite phase again. Therefore, in order to remove the calcite phase, carbon components should be removed first. The lime phase was formed when CO2 was removed from the calcite phase, while the portlandite phase was formed by the introducing of H2O to the lime phase. Therefore, the order in which each phase formed could be in the order of calcite, lime, and portlandite. The reason for the simultaneous presence of the portlandite phase and the lime phase is that the hydroxyl group (OH−) introduced by H2O was not removed completely due to low temperature and/or insufficient heating time. When the sufficient temperature (900°C) and heating time (60 min) were applied, the hydroxyl group (OH−) was removed to transform into lime phase. Since the precursor contained the hydrogen component, it could be possible that the moisture (H2O) and/or the hydroxyl group (OH−) were introduced during the heat treatment process.