GIXD (grazing incidence x-ray diffraction) as a tool for the in situ investigation of electrochemical reactions of metals in electrolyte solutions: The lead electrode in 5M sulphuric acid

GIXD (grazing incidence X-ray diffraction) were performed using a conventional diffractometer (Seifert XRD 3000 TT) for the in situ characterization of the oxidation and reduction reactions on lead electrode surfaces in 5 M aqueous sulfuric acid, During the galvanostatic oxidation, the growing process of lead sulphate (PbSO4) and the further oxidation of PbSO4 to lead dioxide (PbO2) were investigated. Beside the main products PbSO, and beta-PbO2, small amounts of basic lead oxide (3PbO.H2O) and alpha-PbO2 are detectable. The galvanostatic reduction reaction of PbO2 proceeds via PbSO, as an intermediate product to metallic lead.