Micrometer-Precise Determination of the Thin Electrolyte Layer of a Spectroelectrochemical Cell by Microelectrode Approach Curves.

A spectroelectrochemical cell is presented that allows investigations of electrochemical reactions by means of attenuated total reflection infrared (ATR-IR) spectroscopy. The electrode holder for the working (WE), counter and reference electrode as mounted in the IR spectrometer cause the formation of a thin electrolyte layer between the internal reflection element (IRE) and the surface of the WE. The thickness of this thin electrolyte layer (d) was estimated by performing a scanning electrochemical microscopy-(SECM) like approach of a Pt microelectrode (ME), which was leveled with the WE toward the IRE surface.

Integrated scanning Kelvin probe-scanning electrochemical microscope system: development and first applications.

The integration of a scanning Kelvin probe (SKP) and a scanning electrochemical microscope (SECM) into a single SKP-SECM setup, the concept of the proposed system, its technical realization, and first applications are presented and discussed in detail. A preloaded piezo actuator placed in a grounded stainless steel case was used as the driving mechanism for oscillation of a Pt disk electrode as conventionally used in SECM when the system was operated in the SKP mode. Thus, the same tip is recording the contact potential difference (CPD) during SKP scanning and is used as a working electrode for SECM imaging in the redox-competition mode (RC-SECM).