(1. 河北工业大学 材料学院,天津 300130;
2. 河北理工大学 材料学院,唐山 063009;
3. 河北理工大学 化工与生物技术学院,唐山 063009)
摘 要: 在850 ℃的CaCl2熔盐中,以烧结后的Co3O4-SnO2片体为阴极,高纯石墨棒为阳极,采用恒电压电解,制备CoSn合金,研究烧结温度、电解时间对电解过程的影响。采用电子扫描显微镜(SEM)和X射线衍射仪(XRD)分析样品的微观形貌和电解产物的相组成,并采用循环伏安法研究其反应机理。结果表明:经850 ℃烧结的混合氧化物试样,在2.1 V工作电压下电解12 h,可制备出海绵状纯相的CoSn合金。在电脱氧过程中,单质Co首先分步还原,锡的氧化物与熔盐反应后在单质Co表面还原,形成CoSn合金。
关键字: 电脱氧;CoSn;氧化物;熔盐
(1. College of Materials, Hebei University of Technology, Tianjin 300130, China;
2. College of Materials, Hebei Polytechnic University, Tangshan 063009, China;
3. College of Chemical Engineering and Biotechnology, Hebei Polytechnic University, Tangshan 063009, China)
Abstract:The CoSn alloy was prepared in molten CaCl2 at 850 ℃ by constant voltage (2.1 V) electrolysis using sintered pellet of SnO2 and Co3O4 mixture as cathode and pure graphite rod as anode. The effects of the sintering temperature and electrolysis time on the electro-deoxidization process were studied. The morphologies and phases composition of products of the electro-deoxidization were examined by SEM and XRD, respectively. The mechanism of the electro-deoxidization process was studied by cyclic voltammetry. The results show that that pure spongy CoSn can be prepared by direct electrochemical electrolysis of Co3O4/SnO2 mixture pellets sintered at 850 ℃ in molten CaCl2 at 2.1 V for 12 h. During the electro-deoxidization process, in the mixed oxide, Co3O4 is realuced to Co step by step, followed by the reaction of Sn oxide with molten on the surface of the newly-formed Co to form CoSn alloy.
Key words: electro-deoxidization; CoSn; oxide; molten salt