Electrochemical synthesis of octahedral nanostructured PbF₂

In this work, we investigate anodization of Pb in ethylene glycol containing small amount of NH₄F, demonstrating that β-PbF ₂ particles with octahedral morphology can be prepared by adjusting the applied potential and anodizing time. FE-SEM images and XRD measurements of anodic nanostructures as a function of anodizing time clearly show that PbO is first formed on Pb. Subsequently, a local dissolution of PbO leads to formation of skeleton structure of PbO, releasing Pb²⁺ ions in the electrolyte. The lead ions can be precipitated on the walls or intersection of the skeleton walls when the concentration of lead ions is saturated. The method described in this article shows the feasibility of formation of metal fluoride crystal by anodization of metal in a fluoride containing solution.