The Palladium-Nickel Alloy Micro/nano-structures were prepared by electrodeposition. Scanning electron microscopy (SEM) study revealed that the Pd-Ni alloy material exibited quasi one-dimensional tree branch array, line array and quasi two-dimensional compact membrane. Quasi one-dimensional micro/nano structures were about 300 nm in diameter. EDX study results showed that the Ni, Pd atomic ratio is 1.7 : 1, and fraction of Ni (wt%) in the mass was approximately 36%. The quasi two-dimensional compact membrane had periodic configuration. The formation mechanism of such morphologys were proposed. The experiment process and its results reveal revealed Electrolyte solution concentration and growth voltage were crucial for the morphology of deposited products. Our results demonstrate that electrodeposition is a promising method to prepare alloy micro/nano-structures with advantages such as easy to operate, controllable pattern and composition, low cost and large-scale preparation. (C) 2013 The Electrochemical Society. All rights reserved.