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This dissertation, Synthesis and Characterization of Lead Compounds in Waste Lead Battery Treatment by Hengrui, Zhou, 周恆瑞, was obtained from The University of Hong Kong (Pokfulam, Hong Kong) and is being sold pursuant to Creative Commons: Attribution 3.0 Hong Kong License. The content of this dissertation has not been altered in any way. We have altered the formatting in order to facilitate the ease of printing and reading of the dissertation. All rights not granted by the above license are retained by the author. Abstract: Abstract of thesis entitled Synthesis and Characterization of Lead Compounds in Waste Lead Battery Treatment Submitted by Zhou Hengrui for degree of Master of Philosophy at The University of Hong Kong in 2015 The disposal of waste lead-acid batteries has become a global challenge due to the negative effect of lead pollution to environment and human. The traditional pyrometallurgical treatment for waste lead-acid batteries is under severe criticism for the high energy consumption and sulfuric oxide emission. This study investigated the feasibility of alternative treatment methods to prevent the adverse environmental impact created by conventional treatments. The final goal also aimed to beneficially regenerate products with an improved energy storage capacity from waste lead-acid batteries. The study firstly developed a rapid and low-cost hydrometallurgical process to synthesize submicron PbO particles in the presence of polyvinylpyrrolidone (PVP). Secondly, a urea-assisted hydrothermal method and a wet-chemical synthesis method were adopted to fabricate nanostructured PbO and hexagonal disk Pb (CO ) (OH) . 3 3 2 2 i Product phases and microstructures were studied by X-ray diffraction (XRD) and scanning electronic microscopy (SEM). Furthermore, the applications of these products for battery anodes were also examined. The results showed that submicron PbO particles were successfully synthesized via the thermal decomposition of PVP/Pb(CH COO) . The prepared product was 3 2 identified to be orthorhombic β-PbO by qualitative XRD analysis, of which the average particle size was about 200 nm. The critical procedure to form single phase submicron PbO was identified as heat treating the PVP/Pb(CH COO) mixtures with 3 2 a molar ratio of 2 at 550 C for 3 h. The PVP dosage affects the interaction between 2+ Pb and PVP molecule, and this was revealed by the FT-IR spectroscopy results. By a urea-assisted hydrothermal treatment method, nanostructured PbO can be readily recovered from the lead chloride (PbCl ) precursor. The hydrothermal treatment at 150 C for 2 h was efficient to prepare single phase PbCO of which the subsequent 3, calcination was initiated from 350 C for 1 h to yield nanostructured PbO. With a wet-chemical synthesis route, the formation of hydrocerussite (Pb (CO ) (OH) ) 3 3 2 2 started from pH 8 to pH 10. When hydrothermally heated at 180 C for 2.5 h, Pb (CO ) (OH) hexagonal disks were obtained in about 5 m in diameter. 3 3 2 2 Pb (CO ) (OH) rings coexisted at pH 9 to pH 10, and PbO sheets over 10 m were 3 3 2 2 generated from pH 11 to pH 12. The ring shape was a new finding for the hydrocerussite products. The obtained submicron PbO, nanostructured PbO and Pb (CO ) (OH) samples were 3 3 2 2 applied in the lab-scale lead-acid batteries to evaluate the energy storage applications. In comparison, the as-received PbO sample discharged 66 mAh/g at a current of 50 mA/g. The submicron PbO sample showed an enhanced electrochemical property of ii 159 mAh/g at a current of 50 mA/g. The nanostructured PbO sample showed the highest discharge capacity 209 mAh/g at the same current rate. Moreover, the obtained Pb (CO ) (OH) sample revealed an unexpectedly stable discharge 3 3 2 2 performance, with a capacity up to 144 mAh/g. Overall, this study has demonstrated the success of forming lead oxide and hydroce

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