物理化学学报 >> 2006, Vol. 22 >> Issue (11): 1361-1366.doi: 10.1016/S1872-1508(06)60068-5

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水合高氯酸盐+有机溶剂体系中氢氧化物电沉积的EQCM研究

彭谢兰;谢青季;康青;姚守拙   

  1. 湖南师范大学化学化工学院, 化学生物学及中药分析省部共建教育部重点实验室, 长沙 410081
  • 收稿日期:2006-05-23 修回日期:2006-07-06 发布日期:2006-11-06
  • 通讯作者: 谢青季 E-mail:xieqj@hunnu.edu.cn

EQCM Study on the Electrodeposition of Hydroxides in Hydrated Perchlorate + Organic Solvent Systems

PENG Xie-Lan;XIE Qing-Ji;KANG Qing;YAO Shou-Zhuo   

  1. Key Laboratory of Chemical Biology and Traditional Chinese Medicine Research, Ministry of Education, College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, P. R. China
  • Received:2006-05-23 Revised:2006-07-06 Published:2006-11-06
  • Contact: Xie Qing-Ji E-mail:xieqj@hunnu.edu.cn

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摘要： 采用电化学石英晶体微天平(EQCM)定量研究了含水合高氯酸盐的丙酮、DMF、DMSO、C2H5OH或CH3OH有机溶液中LiOH(或NaOH)的电沉积过程. 这种电沉积现象可归因于有机溶液中的溶解氧和共存水在负电位下电还原产生OH−, OH−与溶液中金属阳离子结合生成在非水溶剂中溶解度很小的氢氧化物而沉淀在电极表面, 从而引起压电参数的响应, 而使用四丁基溴化铵为支持电解质时这种现象不明显. 讨论了不同支持电解质、不同溶剂、支持电解质浓度和外加水浓度对氢氧化物电沉积的影响, 估算了氢氧化物沉淀的电极收集效率.

关键词: 非水体系EQCM研究, 丙酮, 水合高氯酸盐, 溶解氧和共存水的电还原, LiOH(或NaOH)的电沉积

Abstract: The electrochemical quartz crystal microbalance (EQCM) method was used to quantitatively examine the precipitation of LiOH (or NaOH) onto a gold electrode at potentials negative to ca −0.8 V (vs SCE) during the cathodic sweep reduction of dissolved oxygen and coexisting water in acetone, DMF, DMSO, C2H5OH, or CH3OH containing hydrated perchlorate, as a result of the poor solubility of electrogenerated hydroxide in the nonaqueous medium. In contrast, the EQCM response indicative of precipitate adherence was negligibly small, when tetrabutyl ammonium bromide was used as supporting electrolyte. Effects of electrolyte and its concentration, solvent, and water content on the electrodeposition of hydroxide were discussed, and the electrode-collection efficiency for the precipitate was evaluated.

Key words: EQCM study on nonaqueous systems, Acetone, Hydrated perchlorate, Reduction of dissolved oxygen and coexisting water, LiOH (or NaOH) electrodeposition