The heat treatment of serpentines for mineral carbonation was studied systematically. Crystallographic, spectroscopic and thermochemical properties were investigated for serpentines before and after heat treatment. Drastic weight loss due to the removal of hydroxy groupe(-OH) occupied in serpentine crystalline was revealed after heat treatment. In XPS results, MgO was founded at heat treated serpentine powders while Mg(OH) was observed at untreated serpentine powders. Metallic oxides originated from serpentine ingredients were regenerated by heat treatment.