本文采用循环伏安一步共聚法在碳纳米管(CNTs)修饰的铂基底上制备了聚苯胺/铁氰化镍(PANI/NiHCF)纳米复合颗粒. 通过电化学石英晶体微天平(EQCM)技术检测了复合颗粒制备过程的质量改变量，并用扫描电镜(SEM)、透射电镜(TEM)和傅立叶变换红外光谱(FTIR)分析了复合颗粒的微观形貌和组成. 结合循环伏安法和EDS能谱考察了该复合电极对Cd²⁺离子的交换性能. 结果表明，三维多孔的CNTs不仅可促进复合颗粒的沉积，而且其独特的网络结构和表面特性对形成PANI/NiHCF复合颗粒的立方体构型起至关重要的作用. 该复合电极在0.1 mol·L^-1 Cd(NO₃)₂溶液中显示了良好的电活性，对Cd²⁺离子有可逆的离子交换性能，通过电控离子交换法可实现废水中Cd²⁺离子的高效分离.

The PANI/NiHCF nanocomposite particles were synthesized on the CNTs-modified Pt substrate by one-step co-polymerization using cyclic voltammetry. Electrochemical quartz crystal microbalance (EQCM) technique was adopted to investigate the polymerization process of the nanocomposite particles and the mechanism of ion exchange in aqueous solution containing Cd²⁺． The morphology and structure of the as-prepared composite particles were characterized by scanning electron microscope (SEM), transmission electron microscope (TEM), and Fourier transform infrared spectroscopy (FT-IR). Combined with cyclic voltammetry (CV) and energy dispersive spectroscopy (EDS), the electrochemical behavior and the mechanism of ion exchange were also investigated in electrolytes of Cd²⁺. Experimental results indicated that the cubic nanocomposite particles of PANI/NiHCF were formed and distributed uniformly on the CNTs substrate. The particles exhibited good electroactivity and reversible electrochemical behavior in aqueous solution containing Cd²⁺, and the Cd²⁺ ions could be separated from aqueous solutions by ESIX processes.