Morphology Dynamics of Single-Layered Ni(OH)₂/NiOOH Nanosheets and Subsequent Fe Incorporation Studied by in Situ Electrochemical Atomic Force Microscopy

Nickel (oxy)­hydroxide-based (NiO_xH_y) materials are widely used for energy storage and conversion devices. Understanding dynamic processes at the solid–liquid interface of nickel (oxy)­hydroxide is important to improve reaction kinetics and efficiencies. In this study, in situ electrochemical atomic force microscopy (EC-AFM) was used to directly investigate dynamic changes of single-layered Ni­(OH)₂ nanosheets during electrochemistry measurements. Reconstruction of Ni­(OH)₂ nanosheets, along with insertion of ions from the electrolyte, results in an increase of the volume by 56% and redox capacity by 300%. We also directly observe Fe cations adsorb and integrate heterogeneously into or onto the nanosheets as a function of applied potential, further increasing apparent volume. Our findings are important for the fundamental understanding of NiO_xH_y-based supercapacitors and oxygen-evolution catalysts, illustrating the dynamic nature of Ni-based nanostructures under electrochemical conditions.