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Triple-layered Ag@Co@Ni core-shell nanoparticles (NPs) containing a silver core, a cobalt inner shell, and a nickel outer shell were formed by an in situ chemical reduction method. The thickness of the double shells varied with different cobalt and nickel contents. Ag0.04@Co0.48@Ni0.48 showed the most distinct core-shell structure. Compared with its bimetallic core-shell counterparts, this catalyst showed higher catalytic activity for the hydrolysis of NH3BH3 (AB). The synergetic interaction between Co and Ni in Ag0.04@Co0.48@Ni0.48 NPs may play a critical role in the enhanced catalytic activity. Furthermore, cobalt-nickel double shells surrounding the silver core in the special triple-layered core-shell structure provided increasing amounts of active sites on the surface to facilitate the catalytic reaction. These promising catalysts may lead to applications for AB in the field of fuel cells. [ABSTRACT FROM AUTHOR]