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In this paper, we report the electrosynthesis and characterization of individual, shape-controlled Pt nanocrystals (NCs) electrodeposited on carbon nanoelectrodes (CNEs). Single Pt NCs were deposited onto the CNEs using an empirically developed square-wave potential program. Characterization by scanning electron microscopy indicates that the sizes of Pt NCs are remarkably reproducible (relative standard deviation = 6%). Electrochemically active surface areas, determined by Cu underpotential deposition and H adsorption/desorption analyses, are also reproducible. Selected area electron diffraction indicates that each Pt NC is comprised of just one single crystal (no grain boundaries). Although different square-wave potential programs lead to different types of crystals, the Pt NCs discussed here have a concave hexoctahedral geometry bound primarily by {13 6 2} surface facets. The results in this report represent a first step toward our ultimate goal of studying electrocatalysis at individual, shape-controlled, single-crystal nanoparticles.

This article provides a summary of the Faraday Discussion on single entity electrochemistry held in York, U.K., in early September, 2016. The introduction provides some context for thinking about electrochemical studies of single entities. The next four sections follow the themes of the meeting as they relate to single-entity electrochemistry: (1) nanoparticles, nanotubes, and nanowires; (2) nanopores and nanofluidics; (3) complex surfaces and reactions at the nanoscale; and (4) molecular electroanalysis. Each paper presented at the Discussion is summarized, and some personal thoughts as to the significance of the findings, the technical advances that made the experiments possible, and common themes between articles are interspersed. Finally, at the end, I round-up my impressions and provide them in a succinct list.