(浙江工业大学 化学工程与材料学院，杭州 310014)
摘 要: 在含As3+和Sb3+的盐酸水溶液中通过恒电流沉积制备砷锑合金。利用循环伏安、计时电流暂态技术研究阴极的电结晶过程，结合SEM和EDS观察分析沉积物的表面形貌及成分。结果表明：在该体系中，AsH3气体的析出得到有效抑制；Sb3+的加入有利于合金的电沉积；砷锑在玻碳电极上的电结晶遵循液相传质控制的三维生长机理，随着Sb3+浓度的增大以及柠檬酸络合剂的加入，其形核速率增大，沉积物晶粒细小；增加酸度可进一步细化晶粒，但酸度过高将产生粉末状沉积物。锑离子浓度的增大或柠檬酸络合剂的加入均导致沉积层中砷含量的减少。
关键字: 盐酸体系；电沉积；砷锑合金；电结晶
（College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China）
Abstract:AsSb alloy was prepared by electrodeposition in hydrochloric acid solution system containing As3+ and Sb3+. The electrocrystallization process in cathode was studied by cyclic voltammetry and chronoamperometric transient method. The surface morphology and the composition of deposits were characterized by SEM and EDS analysis. The results show that the evolution of arsine is restrained in this system. The addition of Sb3+ is beneficial to the electrodeposition of alloy. The electrocrystallization process in glassy carbon electrode follows the diffusion-controlled and three-dimensional nucleation mechanism. The nucleation rate increases with adding citric acid and the Sb3+ concentration increasing, which leades to grains finer. The increase of acidity also increases the nucleation rate, while the powdery deposits would be produced in high acidity. The content of arsenic in deposits reduces with the increase of Sb3+ concentration or the addition of citric acid.
Key words: hydrochloric acid system; electrodeposition; AsSb alloy; electrocrystallization
