We report here the evolution of zinc based high purity phases with novel morphologies such as Zn3N2 hollow structures, ZnO nanowires and nanopowders, as well as metallic Zn layered hexagonal microparticles at progressively increased reaction temperature of 600 degrees C, 700 degrees C, 800 degrees C under NH3 gas atmosphere using Zn powder precursor and keeping all other experimental parameters unchanged. Growth mechanism for Zn3N2 obtained by nitridation, ZnO by oxidation and Zn microparticles via thermal evaporation & condensation process are discussed briefly. The as-synthesized products were characterized by Xray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS) and scanning electron microscopy (SEM). Photoluminescence (PL) studies have revealed very interesting and infrequently observed emission bands at 378 and 661 nm for Zn3N2, 359 and 396 m for ZnO as well as 389 nm for Zn polyhedral microparticles. (C) 2011 Elsevier B.V. All rights reserved.