Abstract
This chapter investigates the processes of adsorption and electrocatalysis, by using differential electrochemical mass spectrometry (DEMS) and scanning tunneling microscope (STM). The use of well-defined single crystals leads to the knowledge of the surface structure. It is a prerequisite for the elucidation of the arrangement of stable adsorbates and intermediates. Bimetallic electrocatalysts show a catalytic activity which is superior to that of their components. Ex situ techniques are employed to determine the surface composition of Pt–Ru electrodes. Ordered bimetallic surfaces formed in ultrahigh vacuum (UHV) help in understanding the role of geometric and electronic effects. DEMS is popular as it provides information on adsorbed species and furthermore on the reaction products and intermediates in a short timescale. The ultimate technique required for the preparation of regularly stepped surfaces consists of cleaning, annealing, and characterization in UHV using Auger electron spectroscopy and low-energy electron diffraction (LEED), followed by a transfer into the electrochemical cell. Hydrogen adsorption peaks are very specific for the local adsorption site geometry. Preferential deposition leads to the suppression of the characteristic hydrogen adsorption peaks. DEMS allows the quantification of the amount of adsorbed organic species by defined potential-induced desorption reactions.
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