The optimization of electrodes for electrocatalysis is critical to the efficient operation of energy conversion applications, i.e., performance and efficiency can be improved by optimizing their fabrication process [1]. In the surface microstructure of anodes has been recognized as a fundamental aspect influencing their functionality [2]. Consequently, it is vital to precisely characterize the microstructure of electrodes. Atomic force microscopy (AFM) has demonstrated to be a potent technique for scrutinizing the nanoscale microstructure of anodes. Nevertheless, AFM has limitations in investigating vast areas, thereby posing a challenge when evaluating the surface microstructure of large-scale electrodes.In this study, we developed a multi-stage data quantification method to overcome the limitations of AFM to measure large electrode areas. The efficacy of the developed approach that combines statistical analysis and computer vision techniques was validated by scrutinizing anodes made under various spray coating process conditions. The results demonstrated that the proposed method facilitated the in-depth evaluation of the degree of homogeneity, surface smoothness, and the presence of cracks or defects, thereby enabling a comprehensive assessment of electrode quality. It was possible to establish structure-performance relationships and delineate the interdependence between surface morphology and anode performance, activity, and cycling stability by combining surface analysis measurements with electrochemical analysis.In conclusion, this link between surface and electrochemical analysis will provide critical insights into anode performance and, in turn, drive the development of advanced materials for energy conversion technologies. Therefore, we believe our method has a high potential to expand the material scientist's toolkit and extend its application to analyze the micro/nanostructure of diverse materials in a wide range of applications, providing novel insights for their optimization. References Siegmund, D., et al., Crossing the valley of death: from fundamental to applied research in electrolysis. Jacs Au, 2021. 1(5): p. 527-535.Chatenet, Marian, et al. "Water electrolysis: from textbook knowledge to the latest scientific strategies and industrial developments." Chemical Society Reviews (2022).
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