Scanning tunnelling microscopy and atomic force microscopy are important tools to investigate solid surfaces at the atomic level in real time both ex-situ and in-situ. These techniques are very useful in Electrochemistry and Electrocatalysis to characterize solid electrode surfaces at the atomic level; to study surface reconstruction at single crystal surfaces; to follow the evolution of surface defects such as steps, vacancies; to investigate adsorption processes at localized domains. This chapter deals with a brief description of fundamental aspects of STM and AFM, including instrumentation, and their application to study Au(111) substrates at the Au(111)/solution interface under different applied potentials; to investigate the structure of self-assembled alcanethiol monolayers adsorbed on Au(111) and C(0001). Changes occurring inter- and intra-adsorbate domains reveal the complexity of these adsorbed monolayers that can only be discovered by local sequential imaging at the molecular level. Finally, the well-known model system for molecular adsorption in Electrochemistry. Au(111)/pyridine aqueous acid solution interface, is described. The correlation between atomic and molecular level information and topography allows us to interpret adsorption data from irregular solid surfaces with a high effective area.
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