A two-stage approach that combines electrodeposition with redox replacement has been used to deposit Pt/Pb nanoparticles on fluorine doped tin oxide (FTO) glass. The deposition takes place by cycling between the two steps in a single electrolyte bath containing both Pb 2+ and Pt 2+ ions. In the first step, Pb is electrodeposited on FTO glass at a potential E 1 and in the second step, Pt replaces the sacrificial Pb directly on the surface at open circuit conditions until the open circuit potential reaches a value E 2 . This method allows a quick deposition of Pt/Pb nanoparticles on FTO glass and the effects of E 1 and E 2 on the Pt/Pb formation and nanoparticle coverage of the surface were studied with SEM and XPS.