title: Solid oxide membrane-assisted controllable electrolytic fabrication of metal carbides in molten salt.
abstract: Silicon carbide (SiC), titanium carbide (TiC), zirconium carbide (ZrC), and tantalum carbide (TaC) have been electrochemically produced directly from their corresponding stoichiometric metal oxides/carbon (MOx/C) precursors by electrodeoxidation in molten calcium chloride (CaCl2). An assembled yttria stabilized zirconia solid oxide membrane (SOM)-based anode was employed to control the electrodeoxidation process. The SOM-assisted controllable electrochemical process was carried out in molten CaCl2 at 1000 °C with a potential of 3.5 to 4.0 V. The reaction mechanism of the electrochemical production process and the characteristics of these produced metal carbides (MCs) were systematically investigated. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses clearly identify that SiC, TiC, ZrC, and TaC carbides can be facilely fabricated. SiC carbide can be controlled to form a homogeneous nanowire structure, while the morphologies of TiC, ZrC, and TaC carbides exhibit porous nodular structures with micro/nanoscale particles. The complex chemical/electrochemical reaction processes including the compounding, electrodeoxidation, dissolution-electrodeposition, and in situ carbonization processes in molten CaCl2 are also discussed. The present results preliminarily demonstrate that the molten salt-based SOM-assisted electrodeoxidation process has the potential to be used for the facile and controllable electrodeoxidation of MOx/C precursors to micro/nanostructured MCs, which can potentially be used for various applications.
authors.affiliation: State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China. xinglizou@shu.edu.cn luxg@shu.edu.cn and Shanghai Key Laboratory of Advanced Ferrometallurgy, Shanghai University, Shanghai 200072, China.
authors.forename: Xingli
authors.initials: X
authors.lastname: Zou
authors.affiliation: State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China. xinglizou@shu.edu.cn luxg@shu.edu.cn and Shanghai Key Laboratory of Advanced Ferrometallurgy, Shanghai University, Shanghai 200072, China.
authors.forename: Kai
authors.initials: K
authors.lastname: Zheng
authors.affiliation: State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China. xinglizou@shu.edu.cn luxg@shu.edu.cn and Shanghai Key Laboratory of Advanced Ferrometallurgy, Shanghai University, Shanghai 200072, China.
authors.forename: Xionggang
authors.initials: X
authors.lastname: Lu
authors.affiliation: State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China. xinglizou@shu.edu.cn luxg@shu.edu.cn and Shanghai Key Laboratory of Advanced Ferrometallurgy, Shanghai University, Shanghai 200072, China.
authors.forename: Qian
authors.initials: Q
authors.lastname: Xu
authors.affiliation: State Key Laboratory of Advanced Special Steel, Shanghai University, Shanghai 200072, China. xinglizou@shu.edu.cn luxg@shu.edu.cn and Shanghai Key Laboratory of Advanced Ferrometallurgy, Shanghai University, Shanghai 200072, China and Institute of Mathematics and Physics, Aberystwyth University, Aberystwyth, SY23 3BZ, UK.
authors.forename: Zhongfu
authors.initials: Z
authors.lastname: Zhou