Controlled synthesis of bimetallic catalysts has attracted much attention in heterogeneous catalysis because their catalytic activity depends on the size of nanoparticles and hence the methods of synthesis. In this work, one convenient method was proposed, with an aim to control the size and dispersion of bimetallic nanoparticles. In this method, Cu2+ (or Ni2+) configurational ion of hydrotalcites was used as directing reagent, which directed the position and dispersion of the final bimetallic nanoparticles by employing the metal interaction between Cu and Au as the driving force. The size, structure and composition of bimetallic nanoparticles were characterized using techniques of X-ray diffraction (XRD), nitrogen physisorption, X-ray photoelectron spectra (XPS) and scanning transmission electron microscopy (STEM). The mean size of bimetallic AuCu nanoparticles was 2.5 nm, which was 1/4 (Step-impregnation) or 1/10 (Co-impregnation) of that prepared by traditional methods. Even if the loading of Au was increased to 10 wt%, the obtained AuCu nanoparticles were still well dispersed. The catalytic activity of AuCu and AuNi nanoparticles in aerobic oxidation of benzyl alcohol was far higher than those prepared by traditional methods. The mechanism of forming bimetallic nanoparticles was investigated. It was found that the dispersion of Cu2+ (or Ni2+) and the interaction between Cu-0 (or Ni-0) and Au-0 are two key factors affecting the dispersion of AuCu (or AuNi) nanoparticles. [GRAPHICS] .