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Homogeneous CaCO₃ microspheres were controllably synthesized via a simple hydrothermal method without using extraneous additives by Ca(OH)₂ saturated solution reacted with CO₂ storage material (CO₂SM), which was obtained by absorbing CO₂ gas in a system containing equimolar ethylenediamine (EDA) and polyethylene glycol 400 (PEG). Specifically, homogeneous pure vaterite spheres were obtained by using 160 g/L CO₂SM solution at 100 °C and a reaction time of two hours. It is noteworthy that the EDA and PEG, which are released from CO₂SM, have dual functions as a CO₂ absorber and crystal regulator in the process of controlling the crystallization of CaCO₃ crystals.