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

Simple and low-cost electrochemical cells for in-situ X-ray powder diffraction (XPD) at 8.04 keV (CuK alpha) and ex-situ scanning electronic microscope (SEM) with energy dispersive spectroscopy (EDS) on the electrode surfaces are presented. Lead (Pb) and aqueous sulfuric acid (H2SO4) solution (molar concentration of 5.35) were chosen as electrode and electrolyte, respectively. A formation of a crystalline lead sulfate (PbSO4) 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.