Thermal characterization of tetrabasic lead sulfate used in the lead acid battery technology
Abstract The thermal production of 4PbO·PbSO 4 was comprehensively studied and characterized for two syntheses routes, i.e. either heating 3PbO·PbSO 4 ·H 2 O, or a mixture of 4PbO:PbSO 4 , in air to about 700?°C. In the 3PbO·PbSO 4 ·H 2 O approach, the formation of an intermediate amorphous phase occurred at around 210?°C with the loss of H 2 O from the hydrated structure. Formation of 4PbO·PbSO 4 initiated at around 270?°C with predominantly 4PbO·PbSO 4 and 13% residual PbO·PbSO 4 existing at 700?°C. With the synthesis route of mixing a stoichiometric ratio of 4PbO with PbSO 4 , an intermediate phase of PbO·PbSO 4 formed at around 300?°C, before the 4PbO·PbSO 4 phase started to form at around 500?°C. Upon further heating, 4PbO·PbSO 4 was the predominant phase with 8% of PbO·PbSO 4 remaining. Both samples decomposed upon further heating to 850?°C. Powder neutron diffraction studies of the final 4PbO·PbSO 4 products from the two different synthesis routes showed similar crystallographic unit cell lattice parameters with slight differences in the PbO:PbSO 4 contents. This could possibly be linked to differences observed in the microscopic crystallite shapes from the two synthesis routes. Highlights Temperature in-situ powder X-ray diffraction of 4PbO·PbSO 4 by two separate synthesis methods were done. Synthesis route one was thermal degradation of 3PbO·PbSO 4 ·H 2 O. Synthesis route two was thermal reaction of 4PbO with PbSO 4 . The two different routes produced crystals with different shapes and sizes of the final reaction product. Neutron powder diffraction and powder x-ray diffraction showed that the two final products had similar crystallographic characteristics. Graphical abstract [DISPLAY OMISSION]
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- DOI : http://dx.doi.org/10.1016/j.solidstatesciences.2016.11.017
- Elsevier : 저널> 권호 > 논문
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