Sonochemical synthesis and characterization of nano-sized zinc(II) coordination complex as a precursor for the preparation of pure-phase zinc(II) oxide nanoparticles

Abstract

In current study, nanoparticles and single crystals of a Zn(II) coordination complex, [Zn(dmph)I₂](<strong>1</strong>), {dmph=2,9-dimethyl-1,10-phenanthroline(neocuproine)}, have been synthesized by the reaction of zinc(II) acetate, KI and neocuproine as ligand in methanol using sonochemical and heat gradient methods, respectively. The nanostructure of <strong>1</strong> was characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses, and the structure of compound <strong>1</strong> was determined by single-crystal X-ray diffraction. The thermal stability of nano-sized <strong>1</strong> has been studied by thermogravimetric (TG) and differential thermal analyses (DTA). Structural determination of compound <strong>1</strong> reveals the Zn(II) ion is four-coordinated in a distorted tetrahedral configuration by two N atoms from a 2,9-dimethyl-1,10-Phenanthroline ligand and two terminal I atoms. The effect of supercritical condition on stability, size and morphology of nano-structured compound <strong>1</strong> has also been studied. The XRD pattern of the residue obtained from thermal decomposition of nano-sized compound <strong>1</strong> at 600 ^°C under air atmosphere provided pure phase of ZnO with the average particles size of about 31 nm.