Thermal characterization of tetrabasic lead sulfate used in the lead acid battery technology |
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| Affiliation: | 1. Department of Chemistry, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth 6031, South Africa;2. uYilo, e-Mobility Technology Innovation Programme, Nelson Mandela Metropolitan University, PO Box 77000, Port Elizabeth, 6031, South Africa;3. DST-NRF Centre of Excellence in Strong Materials, Materials for Energy Research Group University of the Witwatersrand, Private Bag 3, PO Wits, 2050, South Africa;4. Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, PO Wits, 2050, South Africa;5. Research and Development Division, Necsa SOC. Ltd., PO Box 582, Pretoria 0001, South Africa;6. DST-NRF Centre of Excellence in Strong Materials, Carbides & Cermets Focus Area, University of the Witwatersrand, Private Bag 3, PO Wits, 2050, South Africa;1. Université Grenoble Alpes, INES, F-73375 Le Bourget du Lac, France;2. CEA, LITEN, Department of Solar Technologies, F-73375 Le Bourget du Lac, France;1. Universidad Autónoma de Madrid, Departamento de Química Física Aplicada, C/Francisco Tomás y Valiente 7, 28049 Madrid, Spain;2. Exide Technologies, R&D Centre, 19200 Azuqueca de Henares, Spain;1. R & D, Technology Division, Amara Raja Batteries Limited, Karakambadi 517520, India;2. Department of Mech. Engg., University of South Africa, Johannesburg 1710, South Africa;1. Furukawa Electric Institute of Technology Ltd., Budapest, Hungary;2. Department of Physical Chemistry, Eötvös University, Budapest, Hungary |
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| Abstract: | The thermal production of 4PbO·PbSO4 was comprehensively studied and characterized for two syntheses routes, i.e. either heating 3PbO·PbSO4·H2O, or a mixture of 4PbO:PbSO4, in air to about 700 °C. In the 3PbO·PbSO4·H2O approach, the formation of an intermediate amorphous phase occurred at around 210 °C with the loss of H2O from the hydrated structure. Formation of 4PbO·PbSO4 initiated at around 270 °C with predominantly 4PbO·PbSO4 and 13% residual PbO·PbSO4 existing at 700 °C. With the synthesis route of mixing a stoichiometric ratio of 4PbO with PbSO4, an intermediate phase of PbO·PbSO4 formed at around 300 °C, before the 4PbO·PbSO4 phase started to form at around 500 °C. Upon further heating, 4PbO·PbSO4 was the predominant phase with 8% of PbO·PbSO4 remaining. Both samples decomposed upon further heating to 850 °C. Powder neutron diffraction studies of the final 4PbO·PbSO4 products from the two different synthesis routes showed similar crystallographic unit cell lattice parameters with slight differences in the PbO:PbSO4 contents. This could possibly be linked to differences observed in the microscopic crystallite shapes from the two synthesis routes. |
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| Keywords: | Tetrabasic lead sulfate Tribasic lead sulfate Lead sulfate Lead oxide In-situ temperature X-ray powder diffraction Powder neutron diffraction |
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