In this article, structural transformation in nickel doped zinc oxide nanostructures is reported. The ZnO nanostructures are synthesized with 1-10% of nickel doping through a chemical precipitation method. The undoped and doped nanostructures were systematically investigated employing X-ray diffraction (XRD), transmission and scanning electron microscopy (TEM/SEM), Fourier transform infrared (FTIR) and micro-Raman spectroscopy (mu RS). The wurtzite phase of the material and associated lattice parameters were ascertained through XRD analysis. TEM/SEM images reveal the structural transformation of ZnO nanostructures with variation in nickel doping. The study of vibrational modes of nanostructures at different stages of structural transformation, as performed through FTIR and Raman spectroscopy, assist in deciphering the pivotal role of doping concentration in gradual evolution of nickel doped ZnO structure from nanoparticles to nanorods. (c) 2012 Elsevier Ltd. All rights reserved.