Characterizations of Beta-lead Oxide “Massicot” Nano-particles

The present work objective is to prepare and study beta-lead oxide (β-PbO) “massicot” nano-powders by sol-gel method. The lead oxide nano-powders were synthesized through the reaction of lead diacetate solution and oxalate solution. The thermal stability and characterization of the compound were investigated by thermogravimetric (TGA) and differential scanning calorimetry (DSC) analyses, X-ray powder diffraction (XRD) and Fourier transform infrared (FT-IR) techniques. The morphology and crystallographic structural forms were performed by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The obtained TGA and DSC data indicate that the prepared PbO nano-particles are stable. The XRD, HRTEM and SAED data indicate that a mixture of Pb, litharge (tetragonal PbO), and massicot (orthorhombic PbO) were formed with average crystalline size of about 84 nm. The SAED pattern revealed that the formed nano-particles are β-PbO which it was dominant because the annealing temperature was above 400°C.