Nanostructured catalysts play critical roles in a variety of electrochemical energy conversion systems, but the heterogeneous nature of these materials makes it challenging to understand their reactivity at a fundamental level. Significant variations in particle size, shape, ligand coverage, etc. are always present and complicate the interpretation of experimental results. Studies carried out at individual nanoparticle, while experimentally difficult, can potentially overcome this conceptual drawback, providing clear, detailed relationships between structure and function. Here, a suite of experimental methods is outlined for carrying out rigorous electrocatalytic studies at the single nanoparticle level. The primary tools employed in these methods are electrolyte-filled pipets, and the work presented here shows how these tools can be used to both manipulate the spatial arrangement of individual nanoparticles across an interface and probe their electrocatalytic behavior. These methods, when combined with ex situ structural probes, allow single nanoparticle structure-function relationships to be established in a rigorous, high-throughput manner. The utility of these methods is demonstrated through studies of model electrocatalytic reactions at individual, shape-controlled Au nanoparticles and complex high entropy alloy catalyst systems.

Probing electrocatalytic reactions at individual, well-defined nanoparticle catalysts

ACS Spring 2022

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