Due to its exceptional sensitivity, scanning probe microscopy (SPM) enables detailed interrogation of surfaces and interfaces. However, when correlating spatial information to additional surface measurements (such as current, redox activity, force, electrical potential or conductivity, impedance, thermal mapping, viscoelastic parameters, and more), spatial resolution is often limited. Here, we present the development and demonstrate the utility of an Electrochemical (EC) Cell comprised of a sample stage, liquid cup, and cantilever holder that is housed in an environmentally-controlled sample chamber and may be interfaced with an external potentiostat. This EC Cell is employed on a high-resolution, fast scanning Cypher ES atomic force microscope (AFM) in different measurement modes, and enables detailed characterization of localized, electrochemically-controlled morphologies without sacrifices to spatial resolution (atomic resolution is routinely achieved). These EC-AFM measurements are presented and have bearing on the continued development of more-advanced metrologies such as electrochemical scanning tunneling microscopy (EC-STM), scanning electrochemical microscopy (SECM), electrochemical strain microscopy (ESM), and more.

Figure 1. The EC Cell and sample data. (A) Exploded view of the EC Cell. Top: cantilever holder. Middle: sample chamber. Bottom: liquid cup and sample stage. (B) Zoom view of the bottom of the cantilever holder showing the cantilever, clip, and "dipping" architecture. (C) Zoomed, exploded view of the liquid cup and sample stage assembly, including counter electrode. (D) Calcite atomic lattice, imaged in water with the EC Cell (5 nm scan). (E) Example temperature-modulated cyclic voltammetry study conducted with the EC Cell. (F) Example scan-rate-modulated cyclic voltammetry conducted with the EC Cell. (G) Time series of images collected through the Cypher ES top view optics showing deposition of copper on a gold surface during electrochemical reduction. (H) Cyclic voltammogram of copper deposition/stripping on gold, and series of AFM images (2 μm scan) of a copper crystal during stripping.