Towards Reproducible Fabrication of Nanometre‐Sized Carbon Electrodes: Optimisation of Automated Nanoelectrode Fabrication by Means of Transmission Electron Microscopy

Abstract The reproducible fabrication of nanometre‐sized carbon electrodes poses great challenges. Especially, the field of single entity electrochemistry has strict requirements regarding the geometry of these electrochemical probes. Herein, an automated setup for the fabrication of carbon nanoelectrodes based on the pyrolysis of a propane/butane gas mixture within pulled quartz capillaries by means of a moving heating coil is presented. It is shown that mere electrochemical characterisation with conventional redox mediators does not allow for a reliable assessment of the electrode's geometry and quality. Therefore, high‐throughput transmission electron microscopy is used in parallel to evaluate and optimise preparation parameters. Control of the latter gives access to three different electrode types: nanopipettes, nanosamplers and nanodisks.