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A novel combination of Surface X‐ray Scattering techniques (SXS), i. e. GISAXS (Grazing‐Incidence Small‐Angle X‐Ray Scattering), XRR (X‐Ray Reflectivity) and SXRD (Surface X‐Ray Diffraction) alongside with simultaneous detection of gaseous products by OLEMS (On‐Line Electrochemical Mass Spectrometry) has been applied to study under operando conditions structure‐activity relationships of a Pt model electrocatalyst. The SXS‐OLEMS combination is able to follow dynamic changes in surface morphology and crystallography during water electrolysis. To showcase the combined SXS‐OLEMS setup for operando studies of electrode transformations, H 2 and O 2 evolution reactions (HER and OER) on a Pt model electrocatalyst and their dependence on type and degree of surface roughening have been investigated.
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Goryachev et al. (2016) studied this question.
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