Abstract: Glassy carbon, meshed Ti and foam-Ni were used as electrodes were prepared by the electrochemical deposition substrate materials and palladium-loaded The effects of substrate materials on electrocatalytic activity were studied. Cyclic voltammetry results revealed that the hydrogen adsorption peak current value on Pd/GC electrode, Pd/Ti electrode and Pd/foam-Ni electrode were - 23.46 mA, - 59.47 mA and - 60.53 mA, respectively. Scanning electron microscope images indicated that the substrate material had an important effect on the codeposited configuration of Pd on electrode surface. The surface of Pd/GC electrode was rhombus configuration, the surface of Pd/Ti electrode was needle-shaped, and that of Pd/foam-Ni electrode was floss film. With lacunaris configuration, foam-Ni and meshed Ti substrate materials possessed larger surface. After the deposit of Pd, more catalytic sites were obtained, and then it could improve the electrocatalytic activity of the electrodes, and make the electrode show a cheerful prospect in electrochemically reductive dechlorination.