Nanometer Scale Scanning Electrochemical Microscopy Instrumentation.

We report the crucial components required to perform scanning electrochemical microscopy (SECM) with nanometer-scale resolution. The construction and modification of the software and hardware instrumentation for nanoscale SECM are explicitly explained including (1) the LabVIEW code that synchronizes the SECM tip movement with the electrochemical response, (2) the construction of an isothermal chamber to stabilize the nanometer scale gap between the tip and substrate, (3) the modification of a commercial bipotentiostat to avoid electrochemical tip damage during SECM experiments, and (4) the construction of an SECM stage to avoid artifacts in SECM images. These findings enabled us to successfully build a nanoscale SECM, which can be utilized to map the electrocatalytic activity of individual nanoparticles in a typical ensemble sample and study the structure/reactivity relationship of single nanostructures.