The effects of altering reaction conditions in synthesis of a novel lead(II) 2D coordination polymer as well as in achieving the same morphologies of lead(II)oxide micro-nano structures via solid-state process. (1st November 2018) - Souri, Bagher
Graphical abstract: Micro and nano-structure of a new Pb(II) two-dimensional coordination polymer was synthesized by a sonochemical method. The new micro and nano-structure was characterized. PbO nanoparticles were obtained by calcination of compound1 at 700 °C under air atmosphere and were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Abstract: One lead(II) coordination polymer compound (CPC) [Pb(L)(NCS)] n (1 ) (2D layer), in which L stands for C5 H4 NCOO {pyridine-3-carboxylate(−) anion}, has been synthesized following two different experimental approaches; branched tube and sonochemical irradiation methods. Independently of the methodology used, the same crystalline phase is obtained for complex. Single crystal X-ray analyses of compound1 showed that Pb 2+ ions are 5-coordinated, and Hirschfeld surface analyses were studied for1, showing the role of sonochemistry to modulate both morphology and dimensions of the resulting crystalline material. In order to study the effects of the solvent and time of reaction on the formation of [Pb(L)(NCS)] n (1 ) CPC, some experiments were designed, and four samples of1 were synthesized by sonochemical process. Less time of reaction resulted in the formation of compound1 mainly like micro-nano rods. With more time of reaction, various morphologies, mainly microhexagonal of1, were obtained. These four samples have been used as new precursors for the preparation of lead(II)oxide micro-nano structures via solid-state thermal decomposition process. Mix morphology, mainly like sphere micro-nano structures of lead(II)oxide could be prepared from1 . These micro-nano structures were characterized by IR spectroscopy, X-ray powder diffraction (XRD) and scanning electron microscopy (SEM).