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Abstract Electrochemical experiments at individual nanoparticles (NPs) can provide new insights into their structure–activity relationships. By using small nanoelectrodes as tips in a scanning electrochemical microscope (SECM), we recently imaged individual surface‐bound 10–50 nm metal NPs. Herein, we introduce a new mode of SECM operation based on tunneling between the tip and a nanoparticle immobilized on the insulating surface. The obtained current vs. distance curves show the transition from the conventional feedback response to electron tunneling between the tip and the NP at separation distances of less than about 3 nm. In addition to high‐resolution imaging of the NP topography, the tunneling mode enables measurement of the heterogeneous kinetics at a single NP without making an ohmic contact with it. The developed method should be useful for studying the effects of nanoparticle size and geometry on electrocatalytic activity in real‐world applications. 

The continuing interest in nanoscale research has spurred the development of nanosensors for liquid phase measurements. These include nanopore-based sensors typically employed for detecting nanoscale objects, such as nanoparticles, vesicles and biomolecules, and electrochemical nanosensors suitable for identification and quantitative analysis of redox active molecules. In this Perspective, we discuss conductive nanopipettes (CNP) that can combine the advantages of single entity sensitivity of nanopore detection with high selectivity and capacity for quantitative analysis offered by electrochemical sensors. Additionally, the small physical size and needle-like shape of a CNP enables its use as a tip in the scanning electrochemical microscope (SECM), thus, facilitating precise positioning and localized measurements in biological systems.