In-situ high-resolution scanning electron microscopy observation of electrodeposition and stripping of lead in an electrochemical cell

A compact electrochemical cell capped with a silicon nitride (SiN) film of 50 nm thick as an electron window was developed for a side-entry holder of a high-resolution scanning electron microscope (SEM). Electrodeposition and stripping of lead (Pb) were examined on a gold electrode formed on the SiN film, which was faced inside the cell filled with an aqueous solution of lead nitrite. The SEM images of growth and dissociation of Pb were recorded simultaneously with cyclic voltammograms, controlled with a two-terminal potentiostat. Particulate growth of Pb at the edge of a gold (Au) electrode was observed at the underpotential deposition of Pb, followed by dendrite growth of Pb at higher deposition potentials. The growth mode changed depending on the edge morphology of the Au electrode. This indicated that in-situ microscopic observation was invaluable for understanding the phenomena of electrodeposition in electrochemistry.