(浙江工業(yè)大學 化學工程與材料學院，杭州 310014)
摘 要: 在含As3+和Sb3+的鹽酸水溶液中通過恒電流沉積制備砷銻合金。利用循環(huán)伏安、計時電流暫態(tài)技術研究陰極的電結晶過程，結合SEM和EDS觀察分析沉積物的表面形貌及成分。結果表明：在該體系中，AsH3氣體的析出得到有效抑制；Sb3+的加入有利于合金的電沉積；砷銻在玻碳電極上的電結晶遵循液相傳質控制的三維生長機理，隨著Sb3+濃度的增大以及檸檬酸絡合劑的加入，其形核速率增大，沉積物晶粒細小；增加酸度可進一步細化晶粒，但酸度過高將產(chǎn)生粉末狀沉積物。銻離子濃度的增大或檸檬酸絡合劑的加入均導致沉積層中砷含量的減少。
關鍵字: 鹽酸體系；電沉積；砷銻合金；電結晶
（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
