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      Electrochemical Scanning Probe Microscopies in Electrocatalysis

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          Abstract

          Improvements toward highly efficient electrochemical energy conversion require a detailed understanding of the underlying electrochemical processes at electrified solid–liquid interfaces. In situ and in operando studies by means of electrochemical scanning probe microscopy (EC‐SPM) have become indispensable experimental tools due to their capability of resolving surface topography down to the atomic level even within the harsh environment of electrolytes. EC‐SPM methodologies have thus contributed tremendously to the current understanding of electrocatalysis. In this review article, recent achievements in complementary EC‐SPM techniques, namely electrochemical scanning tunneling microscopy (EC‐STM), electrochemical atomic force microscopy (EC‐AFM), scanning electrochemical potential microscopy (SECPM), and scanning electrochemical microscopy (SECM), are discussed with particular focus on electrochemical phenomena important for the field of electrocatalysis. The currently available options for obtaining insight on local chemical composition and local reactivity as well as important electrocatalytic model systems are considered. In addition, the application of EC‐SPM methods to metal ion batteries is addressed.

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          Atomic Force Microscope

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            Origin of the Overpotential for Oxygen Reduction at a Fuel-Cell Cathode

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              Identification of active edge sites for electrochemical H2 evolution from MoS2 nanocatalysts.

              The identification of the active sites in heterogeneous catalysis requires a combination of surface sensitive methods and reactivity studies. We determined the active site for hydrogen evolution, a reaction catalyzed by precious metals, on nanoparticulate molybdenum disulfide (MoS2) by atomically resolving the surface of this catalyst before measuring electrochemical activity in solution. By preparing MoS2 nanoparticles of different sizes, we systematically varied the distribution of surface sites on MoS2 nanoparticles on Au(111), which we quantified with scanning tunneling microscopy. Electrocatalytic activity measurements for hydrogen evolution correlate linearly with the number of edge sites on the MoS2 catalyst.
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                Author and article information

                Contributors
                (View ORCID Profile)
                Journal
                Small Methods
                Small Methods
                Wiley
                2366-9608
                2366-9608
                August 2019
                November 14 2018
                August 2019
                : 3
                : 8
                Affiliations
                [1 ] Physik‐Department ECS Technische Universität München James‐Franck‐Str. 1 85748 Garching Germany
                [2 ] Institut für Informatik VI Technische Universität München Schleißheimerstrasse 90a 85748 Garching Germany
                Article
                10.1002/smtd.201800387
                65ef634c-aac1-473b-b3b3-4bfbc6d88f45
                © 2019

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