Impacts of Forced Convection Generated via High Precision Stirring on Scanning Electrochemical Microscopy Experiments in Feedback Mode

Abstract

In this study, the effects of forced convection on scanning electrochemical microscopy (SECM) experiments in feedback mode using ferrocenemethanol as redox mediator are presented. Forced convection, which enhances the mass transfer inside the system, was generated via an electrical high precision stirrer integrated into the SECM setup. A thin‐film interdigitated array electrode serving as model substrate was investigated with probe scan curves in z‐direction and SECM imaging in constant height mode utilizing ultramicroelectrodes (UME) with diameters (dprobe) of 25 μm and 12.5 μm. It was found that forced convection increased the overall current during SECM imaging without distorting distinctive features of the imaged structure when working with a 25 μm UME at substrate‐to‐tip distances of 14 μm and 11 μm. Furthermore, the electrochemical contrast was improved under hydrodynamic conditions for a substrate‐to‐tip distance of 11 μm and scan rates of 5 μm s−1, 10 μm s−1, 20 μm s−1 and 40 μm s−1. When further decreasing the gap between the UME and the substrate to 9 μm almost no effects of the forced convection were observed. Consequently, for a 25 μm UME, forced convection led to higher currents and improved performance during SECM experiments in feedback mode at substrate‐to‐tip distances of 14 μm and 11 μm, whereas no effects were observed for a 12.5 μm UME at a distance of 8 μm.

Scanning Electrochemical Microscopy of Electrically Heated Wire Substrates

“…To overcome this problem, our group has introduced forced convection into the SECM cell, either by stirring [28] or by a flow of the electrolyte solution [29], resulting in a rapidly established steady-state diffusion layer. In addition, forced convection led to a higher contrast in feedback mode measurements [30].…”

Development of a Temperature‐pulse Enhanced Electrochemical Glucose Biosensor and Characterization of its Stability via Scanning Electrochemical Microscopy

“…Forced convection was introduced into the measurement cells by different means [5], resulting in increased currents and reproducibility of images as stable diffusion layers can be established at the generator electrode. Furthermore, this also led to contrast improvement in feedback mode imaging of SECM due to an enhanced feedback cycle at conductive surfaces [6].…”