Al was prepared by a new method in molten salt at low temperature. Sintered alumina pellets were used as cathode; graphite rod was employed as anode; and the molten CaCl2-NaCl was the electrolyte. A constant 3.2 V voltage was applied in this experiment, and oxygen in solid alumina cathode was reduced by direct electrochemical deoxidation at 550℃. In this process, the current gradually decreased with increasing time and the alumina pellets became grey and porous. The metallic particles were obtained and characterized by XRD (X-ray diffraction) and SEM (scanning electron microscopy).