Spectroscopy and in‐situ X‐ray diffraction analysis on the corrosion process at the interface Pb/H₂SO₄ using a low‐cost electrochemical cell

Abstract

Simple and low-cost electrochemical cells for in-situ X-ray powder diffraction (XPD) at 8.04 keV (CuKα) and ex-situ scanning electronic microscope (SEM) with energy dispersive spectroscopy (EDS) on the electrode surfaces are presented. Lead (Pb) and aqueous sulfuric acid (H 2 SO 4 ) solution (molar concentration of 5.35) were chosen as electrode and electrolyte, respectively. A formation of a crystalline lead sulfate (PbSO 4 ) on the Pb electrode surface with initial precipitation/nucleation at 1 h and a posterior crystal grow (with orthorhombic crystalline structure) on the Pb electrode surface, over the time (from 4 h to 12 weeks) was observed. The result is consistent with the literature, showing the full characterization capability of the proposed cells.