Atomic resolution imaging of electrode surfaces in solutions containing reversible redox species

Procedures are described for insulating metal scanning tunneling microscope (STM) tips with either glass or polymer coatings. In solutions containing 0.10 M of a reversible redox couple, Fe(CN) - 3/-46 , the faradaic limiting current to polymer coated tips was 200–500 pA and that for glass coated tips was <10 pA. For polymer insulated tips, steady-state currents of 10–100 pA were observed at tip-sample displacements less than 0.3 µm. The suppression of faradaic current achieved by these coating procedures enabled the collection of the first atomic resolution STM images of highly ordered pyrolytic graphite electrodes in contact with redox-active electrolytes. Preliminary data for the in situ electrochemical characterization of these tips are also discussed

Design of a scanning tunneling microscope for electrochemical applications

A design for a scanning tunneling microscope that is well suited for electrochemical investigations is presented. The construction of the microscope ensures that only the tunneling tip and the sample participate in electrochemical reactions. The design also allows rapid replacement of the tip or sample, and enables facile introduction of auxiliary electrodes for use in electrochemical experiments. The microscope utilizes stepper motor driven approach mechanics in order to achieve fully remote operation and to allow reproducible coarse control of tip/sample spacings for electrochemical experiments. Highly ordered pyrolytic graphite images at atomic resolution in air and aqueous solutions can be obtained with this microscope