Scanning electrochemical microscopy at variable temperatures

Phys Chem Chem Phys. 2013 Apr 14;15(14):5215-23. doi: 10.1039/c3cp43520b.

Abstract

All chemical reactions are influenced by temperature, however, temperature is usually not considered an important parameter which has to be varied or at least controlled in SECM measurements. A precise temperature-control unit was designed and integrated into a SECM setup which allows setting the temperature of the sample and the adjacent electrolyte in a range between 0 and 100 °C without causing convection. Data acquisition was synchronized with the current pulses through the Peltier element to decrease the noise and keep the tip-to-sample distance constant during imaging. SECM images in the feedback mode, generator collector mode and the redox competition mode for model samples such as an enzyme entrapped within a polymer spot or oxygen reduction catalysts demonstrate the importance of controlling temperature as well as performing SECM experiments at predefined and constant increased temperature.