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Scanning electrochemical cell microscopy (SECCM) is increasingly applied to determine the intrinsic catalytic activity of single electrocatalyst particle. This is especially feasible if the catalyst nanoparticles are large enough that they can be found and counted in post-SECCM scanning electron microscopy images. Evidently, this becomes impossible for very small nanoparticles and hence, a catalytic current measured in one landing zone of the SECCM droplet cannot be correlated to the exact number of catalyst particles. We show, that by introducing a ruler method employing a carbon nanoelectrode decorated with a countable number of the same catalyst particles from which the catalytic activity can be determined, the activity determined using SECCM from many spots can be converted in the intrinsic catalytic activity of a certain number of catalyst nanoparticles.

International audience; Carbon-based nanomaterials are renowned for their exceptional properties, making them propitious candidates for oxygen reduction reaction (ORR) electrocatalysis. However, their intrinsic activity is often challenging to investigate unambiguously with conventional methodologies due to the inherent complexities of such systems and the material itself. Zooming into the material and gaining electrochemical information with high resolution is a way to get rid of many experimental factors that influence the catalytic activity in macro-scale measurements. Herein, we employ nano-scale scanning electrochemical cell microscopy (SECCM) to investigate individual catalyst agglomerates with and without Nafion content. The intrinsic ORR activity of the catalyst was unravelled by using a unique approach of normalizing the data of all measured points by their distinctive electrochemical surface area (ECSA). When coupling with scanning electron microscopy (SEM), the structure and morphology of the catalytically active agglomerateswere visualized

Anatase TiO2 is a promising material for Li-ion (Li+) batteries with fast charging capability. However, Li+ (de)intercalation dynamics in TiO2 remain elusive and reported diffusivities span many orders of magnitude. Here, we develop a smart protocol for scanning electroche-mical cell microscopy (SECCM) with in situ optical microscopy (OM) to enable the high-throughput charge/discharge analysis of single TiO2 nanoparticle clusters. Directly probing active nanoparticles revealed that TiO2 with a size of ~50 nm can store over 30% of the theoretical capacity at an extremely fast charge/discharge rate of ~100 C. This finding of fast Li+ storage in TiO2 particles strengthens its potential for fast-charging batteries. More generally, smart SECCM-OM should find wide applications for high-throughput electrochemical screening of nanostructured materials.