Developing Time-Resolved Synchrotron Infrared Spectroscopy for Spectroelectrochemical Measurements
This thesis details my work in developing spectroelectrochemical platforms utilizing synchrotron infrared radiation (SIR) and time-resolved FTIR to study the kinetics of electrochemical reactions on second to millisecond scale with high chemical sensitivity. It will cover development of spectroelectrochemical cells and procedures compatible with the mid-IR beamline at the Canadian Light Source to study irreversible electrocatalytic processes with rapid scan FTIR in reflection mode. The thesis demonstrates application of SIR-based rapid scan FTIR to spatially map catalytic activity on heterogenous PtNi electrode and provides proof-of-principle for its capability for combinatorial screening for binary electrocatalysts. The thesis discusses the development of time-resolved step scan FTIR in attenuated total reflection - surface enhancing infrared absorption spectroscopy configuration (ATR-SEIRAS) to improve signal-to-noise of the measurement for increased detection limits and time-resolution, before demonstrating the utility of the developed step scan ATR-SEIRAS platform by investigation of the kinetics of conformational changes within self-assembled monolayers (SAM) of ferrocene alkanethiols. Overall, the work described in this thesis outlines the advancement of SIR-based spectroelectrochemical platforms within the group to a point, where they can be directly applied to investigation of dynamics processes within electrochemical reaction.
Electrochemistry, FTIR, IR spectroelectrochemisry
Doctor of Philosophy (Ph.D.)