An electrochemical approach is able to convert low-grade nickel-copper matte (LNCM) to copper-, nickel-, and iron-alloys in both molten NaCl-KCl and MgCl2-NaCl-KCl without sulfur dioxide emissions. Since the LNCM contains the mixture of sulfides and oxides, the electrochemical deoxidation and desulfurization are taking place together, producing alloys in a one-step process. Thermodynamic properties of several sulfides/oxides were analyzed, and the electrochemical reduction behaviors of LNCM were investigated in by cyclic voltammetry (CV) using a powder modified working electrode. The morphologies of the electrolytic products could be tailored by adjusting both operating temperature and cell voltage of the electrolysis. Overall, this paper provides an environment-friendly pathway to comprehensively utilize minerals in molten salts. (C) 2018 The Electrochemical Society.