本文利用电沉积制得ZrO₂掺杂铌基二氧化铅电极，通过扫描电镜（SEM）和X射线衍射（XRD）观察表征了Nb/ZrO₂+PbO₂电极表面形貌特征及组成. 用线性伏安曲线、电化学交流阻抗和循环伏安曲线测试了Nb/ZrO₂+PbO₂电极电化学性能，及其甲基橙（MO）的降解电催化效果. 结果表明，ZrO₂掺杂使Nb/PbO₂电极表面更致密、粗糙，结晶尺寸更小，增大了电极比表面积，提高了电极电催化活性. Nb/ZrO₂+PbO₂电极活性层主要由β-PbO₂和少量的α-PbO₂以及部分ZrO₂共沉积而成. 有较高的析氧电位、吸附电容和较低的电荷转移电阻，其甲基橙（MO）降解电催化活性更佳，降解过程受扩散控制.

The zirconium oxide (ZrO₂)-doped niobium based lead oxide (Nb/PbO₂) electrode was prepared by electrodeposition. The microstructures and electrochemical properties of Nb/ZrO₂+PbO₂ electrode were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), linear sweep voltammetry, electrochemical impedance spectroscopy and cyclic voltammotry. In addition, the Nb/PbO₂ electrode was used as an anode for the electrochemical degradation of methyl orange (MO). Results revealed that the ZrO₂ doping made the Nb/PbO2 electrode surface denser and rougher with smaller sized crystal particles, which increased the specific surface area and enhanced the electrocatalytic activity of the electrode. The Nb/ZrO₂+PbO₂ electrode was mainly composed of β-PbO₂ with a small amount of α-PbO₂ and ZrO₂ formed by codeposition. Accordingly, the Nb/ZrO₂+PbO₂ electrode possessed higher oxygen-evolution potential, larger adsorption capacity and lower charge-transfer resistance, as well as higher electrocatalytic activity in the degradation of organic materials than the Nb/PbO₂ electrode. The MO degradation processes were irreversible and controlled by diffusion.