The objective of this study is to prepare lanthanum and cerium metals by fused salt electrolysis of their anhydrous chloride in molten media such as LiCl-KCl, NaCl-KCl, KCl, NaCl, and LiCl and to characterize the metal deposit by X-ray diffraction, energy dispersive X-ray fluorescence, and inductive coupled plasma-atomic emission spectroscopy. Deposit metal of puritymore than 99 % was obtained in each of the experiments. The entire process starting from preparation of anhydrous lanthanum/cerium chloride to electrolysis yielding of metal deposits has been described. The effect of process parameters such as temperature, electrolyte composition, and current density on the current efficiency was studied. All these parameters were varied to get the highest current efficiency and metal yield. The major non-rare earth impurities with the deposit are found to be Fe, Cr, and Ni along with ～1×10-3 of total gaseous impurities.
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