采用单极脉冲法在铂基体表面一步合成聚苯胺/铁氰化镍 (PANI/NiHCF) 有机-无机杂化膜，并分析了杂化膜高电势静电吸引沉积机理. 高电压聚合杂化膜避免了Fe(CN)₆^3-的还原，并形成单一“不可溶”结构NiHCF. 用扫描电镜（SEM）、X射线能谱仪（EDS）和傅立叶变换红外（FT-IR）光谱研究了杂化膜表面形貌及组成，并考察了不同单极脉冲电压制得杂化膜的电化学性能. 结果表明，单极脉冲电压1.0 V制得的PANI/NiHCF杂化膜有最佳的电活性和良好的稳定性. 使用计时电流法考察了杂化膜电极的过氧化氢（H₂O₂）的电催化还原活性，在0.5 mol·L^-1 KCl + 0.5 mol·L^-1 HCl电解液中，PANI/NiHCF杂化膜电极过氧化氢催化还原电流与其浓度（4.0×10^-4 ~ 1.6×10^-2 mol·L^-1）呈良好的线性关系，相关性系数R = 0.9991，检出限为6.09×10-5 mol·L-1，灵敏度为1075 mA·(mol·L-1)-1·cm-2.

Organic–inorganic hybrid films composed of polyaniline/nickel hexacyanoferrate (PANI/NiHCF) were fabricated on platinum substrates using unipolar pulse one-step electrodeposition. The deposition mechanism of hybrid film was proposed: Due to high potential of unipolar pulse electrodeposition, which avoided the reduction of Fe(CN)₆^3-, the films with high electrocatalytic property and “insoluble” form of NiHCF were achieved. The morphology and composition of PANI/NiHCF hybrid film were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), and Fourier transform infrared spectroscopy (FT-IR). The effect of pulse potential on the electrochemical performance of hybrid film was investigated in detail. Results showed that pulse potential had a major impact on electroactivity and stability of the film, and the optimal deposition potential was 1.0 V. The hybrid ?lms exhibited high electrocatalytic activity, eligible sensitivity and low detection limit in detecting hydrogen peroxide (H2O2). The linear range for the detection of H₂O₂ was from 4.0×10^-4 to 1.6×10^-2 mol·L^-1 with a correlation coefficient of 0.9991, a sensitivity of 1075 mA·(mol·L^-1)^-1·cm^-2 and a detection limit of 6.09×10^-5 mol·L^-1.