The Identification of the Reduction Peak of Tetragonal PbO on Pb by Laser Raman Scattering and X‐Ray Diffraction

The debate about the reaction causing the cathodic peak at about −800 mV on the linear sweep voltammogram of a Pb electrode in solution is still unsettled. In this paper, ex situ laser Raman scattering and in and ex situ x‐ray diffraction techniques are used to identify the peak, which proved to be the reduction of tetragonal according to the changes of the diagnostic diffraction lines with and Raman bands at 148 and 343 cm−1. Electrochemically inert also exists on the Pb surface.