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In situ ellipsometric and electrochemical monitoring of the oxidation of a Pb–Ca–Sn alloy used in the lead acid batteries

Abstract : The oxidation process of the Pb-0.08 wt.% Ca-1.2 wt.% Sn alloy was investigated by in situ spectroscopic ellipsometry measurements, combined with electrochemical measurements. The evolutions of the electrochemical and optical parameters show a mechanism of the film growth in two parts. In the first 10 min, the ellipsometric spectra exhibit large variations, whereas the measured current is approximately 0.3 mA cm−2. During this complex step, the surface topography is continuously changing. This stage corresponds to the growth of lead sulfate crystals, which is then oxidized in a thin and flat PbO2 layer, as confirmed by ex situ X-ray diffraction and scanning electron microscopy analysis. The second part is identified by a rapid and important decrease of the current, down to a low and steady value of approximately 0.01 mA cm−2. At once, the optical spectra vary slightly. A duplex layer model has been used to interpret spectroscopic ellipsometric measurements. The upper layer is likely composed of β-PbO2 as suggested by ex situ X-ray diffraction analysis. This model indicates a total thickness of the film approximately 480 nm at the end of the polarization (24 h).
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https://hal.univ-lorraine.fr/hal-02900547
Contributor : Laurent Broch <>
Submitted on : Thursday, July 16, 2020 - 11:20:29 AM
Last modification on : Thursday, November 12, 2020 - 2:30:09 PM

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N. Stein, G. Bourguignon, L. Raboin, L. Broch, L. Johann, et al.. In situ ellipsometric and electrochemical monitoring of the oxidation of a Pb–Ca–Sn alloy used in the lead acid batteries. Thin Solid Films, Elsevier, 2004, 455-456, pp.735-741. ⟨10.1016/j.tsf.2003.11.259⟩. ⟨hal-02900547⟩

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