Characterization of High‐Surface‐Area Electrocatalysts Using a Rotating Disk Electrode Configuration

A newly developed method is presented which allows the characterization of the electrocatalytic properties of highly dispersed electrocatalysts in a true rotating disk electrode (RDE) configuration by attaching the catalyst powder on a glossy carbon electrode via a thin Nafion film. Complete utilization and high reproducibility of both the electrode preparation and the catalyst loading could be shown via voltammetry and CO stripping voltammetry. Furthermore RDE measurements on the electro‐oxidation of hydrogen on Pt/Vulcan showed that the effect of diffusion through the Nation film can be avoided by proper electrode preparation. Therefore, the electrode kinetics for fuel cell relevant reactions under continuous flow conditions can be measured directly without mathematical modeling.