The present paper describes the synthesis of nanostructure Pd/Au core/shell and study of electric catalysis, control of particle size composition and spins. Oil-bathing thermal decomposition was adopted to prepare the core/shell Pd/Au bimetallic alloy nanoparticles. The PVP and ethylene glycol were used as surfactant and stabilizing agent. Based on the solution concentration, size, and surface adsorption energy and control of the phase, the uniform homogeneous Pd/Au nanostructure was obtained. The experiments measured the HAADF and HRTEM to test the shape of nanostructure and EDS particle distribution. The products were characterized by TEM/XRD and XPS. The results show that Pd/Au nanoparticles have the structure of truncated octahedron different from Au/Pd core/shell. The Pd/Au nanoparticles have the properties of activity, wear, electric catalysis and stability.