In situ AFM visualization of Li–O(2) battery discharge products during redox cycling in an atmospherically controlled sample cell

The in situ observation of electrochemical reactions is challenging due to a constantly changing electrode surface under highly sensitive conditions. This study reports the development of an in situ atomic force microscopy (AFM) technique for electrochemical systems, including the design, fabrication, and successful performance of a sealed AFM cell operating in a controlled atmosphere. Documentation of reversible physical processes on the cathode surface was performed on the example of a highly reactive lithium–oxygen battery system at different water concentrations in the solvent. The AFM data collected during the discharge–recharge cycles correlated well with the simultaneously recorded electrochemical data. We were able to capture the formation of discharge products from correlated electrical and topographical channels and measure the impact of the presence of water. The cell design permitted acquisition of electrochemical impedance spectroscopy, contributing information about electrical double layers under the system’s controlled environment. This characterization method can be applied to a wide range of reactive surfaces undergoing transformations under carefully controlled conditions.