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Synthesis and characterization of nano-peanuts of lead(II) coordination polymer [Pb(qcnh)(NO 3 ) 2 ] n with ultrasonic assistance: A new precursor for the preparation of pure-phase nano-sized PbO



Synthesis and characterization of nano-peanuts of lead(II) coordination polymer [Pb(qcnh)(NO 3 ) 2 ] n with ultrasonic assistance: A new precursor for the preparation of pure-phase nano-sized PbO



Ultrasonics Sonochemistry 34: 255-261



A sonochemical method was used to synthesize nano-peanuts of a new lead(II) coordination 1D polymer, [Pb(qcnh)(NO3)2]n (1), where qcnh=2-quinolincarbaldehyde nicotinohydrazide. The compound was characterized by scanning electron microscopy (SEM), elemental analysis, IR spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray powder diffraction (XRD), and single crystal X-ray analysis. The X-ray structure revealed that the Pb(II) atom is coordinated by one oxygen and three nitrogen atoms from two qcnh ligands and five oxygen atoms from three nitrate ligands in an 8+1 fashion with a PbN3O6 donor set. One of the PdN distances in the vicinity of the central atom is a bit longer (Pb1N1=2.939(4) Å), which shows the effect of the 6s2 lone electron pair localized within the valence shell of the lead(II) atom. PbO nanoparticles were obtained by thermolysis of 1 at 180°C with oleic acid as a surfactant. The average diameter of the nanoparticles was estimated by XRD to be 28nm. The morphology and size of the prepared PbO nanoparticles were further studied using SEM.

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Accession: 058954414

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PMID: 27773243

DOI: 10.1016/j.ultsonch.2016.05.041


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