ZnO/ZnS heterostructure nanorod arrays are fabricated by a two-step electrochemical deposition method from dimethylsulfoxide (DMSO) aqueous solution. The XRD and TEM pattern indicate the ZnO/ZnS nanorods are composed of hexagonal wurtzite ZnS structure and hexagonal wurtzite ZnO structure. The optical and photocatalytic properties of as-prepared ZnO/ZnS are investigated in detail. (C) 2011 The Electrochemical Society. [DOI: 10.1149/1.3597611] All rights reserved.