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An electroactive hybrid film composed of amorphous α-zirconium phosphate and polyaniline (α-ZrP/PANI) is controllably synthesized on carbon nanotubes (CNTs) modified Au electrodes in aqueous solution by cyclic voltammetry method. Electrochemical quartz crystal microbalance (EQCM), scanning electron microscopy (SEM) and X-ray power diffraction (XRD) analysis are applied for the evaluation of the synthesis process. It is found that the exfoliated amorphous α-ZrP nanosheets are well dispersed in PANI and the hydrolysis of α-ZrP is successfully suppressed by controlling the exfoliation temperature and adding appropriate supporting electrolyte. The insertion/release of heavy metals into/from the film is reversibly controlled by a potential-triggered mechanism. Herein, α-ZrP, a weak solid acid, can provide an acidic micro-environment for PANI to promote the electroactivity in neutral aqueous solutions. Especially, the hybrid film shows excellent potential-triggered adsorption of Pb 2+ ion due to the selective complexation of Pb 2+ ion with oxygen derived from P O H of α-ZrP. Also, it shows long-term cycle stability and rapid potential-responsive adsorption/desorption rate. This kind of novel hybrid film is expected to be a promising potential-triggered ESIX material for separation and recovery of heavy metal ions from wastewater. [ABSTRACT FROM AUTHOR]