Perfect polycrystalline NiPb dendrites were prepared via cathodic electrochemical deposition on Cu substrates from aqueous solution. Cyclic voltammetry was used to gain insight into the Ni/Pb codeposition mechanism. The results reveal that the dendrite consists of a long central backbone and very orderly secondary and tertiary branches. The size and shape of the dendritic structures can be tunable by changing the synthetic parameters. A formation mechanism is proposed to illustrate the growth process. (C) 2010 The Electrochemical Society. [DOI:10.1149/1.3462999] All rights reserved.