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The electrochemical behaviors of Al(III) deposits on Ni substrates were investigated in LiCl-KCl-AlCl3 (2 wt.%) molten salts. Various electrochemical methods, including cyclic voltammetry (CV), square wave voltammetry (SWV), and open circuit chronopotentiometry (OCP) were used to explore the deposition processes of Al(III) on Ni substrates. Five kinds of Al-Ni alloys phase were firstly electrodeposited by the regulation of deposition potential form LiCl-KCl-AlCl3 (2 wt.%) molten salts at 753 K. The formation of Al-Ni alloys, such as AlNi3, Ni5Al3, AlNi, Al3Ni2, and Al3Ni were confirmed by X-ray diffractometer (XRD) and the cross-section morphologies were investigated by scanning electron microscope (SEM). Meanwhile, it was found that the temperature of molten salt was another key parameter for the controlling of alloys phase. No Al-Ni alloys phase other than AlNi3 and Ni5Al3 could be deposited at 703 K. [ABSTRACT FROM AUTHOR]