Surfactant-free one-step redox reactions between two types of metal cations enable the synthesis of core-shell nanoparticles without sophisticated control. The reduced noble metal cations form a solid core, and the transition metal cations dissolved upon oxidation induce the subsequent formation of a metal oxide shell. Various nanostructures are obtained from the combination of reduction-preferring Au 3+ , Pd 2+ , Pt 2+ , Rh 3+ , and Ir 3+ cations, and oxidationpreferring Ti 3+ , Mo 3+ , V 2+ , and V 3+ cations. Among the synthesized core-shell nanoparticles, Au-M (M = Ti, Mo, and V) is selected for the photodegradation tests at 365 and 808 nm.