Hybrid scanning electrochemical cell microscopy-interference reflection microscopy (SECCM-IRM): tracking phase...

Area of Science:

• Surface Science and Electrochemistry
• Advanced Microscopy Techniques
• Materials Science and Nanotechnology

Background:

• Studying interfacial processes requires techniques with high spatial and temporal resolution.
• Scanning Electrochemical Cell Microscopy (SECCM) confines reactions to small areas.
• Interference Reflection Microscopy (IRM) offers high surface sensitivity near substrates.

Purpose of the Study:

• To combine SECCM and IRM for real-time, in situ monitoring of interfacial electrochemical processes.
• To track the status of the SECCM meniscus during experiments.
• To investigate surface changes and material precipitation at electrode/electrolyte interfaces.

Main Methods:

• Coupling SECCM with IRM using transparent conductive substrates (e.g., ITO on glass).
• Real-time optical monitoring of the SECCM meniscus and interfacial phenomena.
• Voltammetry, electrowetting quantification, and CaCO3 precipitation studies.

Main Results:

• Demonstrated stability and reproducibility of the SECCM meniscus over a wide potential window (ca. 5% variation).
• Detected and quantified subtle electrowetting at high cathodic potentials.
• Observed surface changes possibly due to indium nanoparticle formation and characterized CaCO3 precipitation patterns.

Conclusions:

• The combined SECCM-IRM technique provides high spatiotemporal resolution for studying interfacial processes.
• This method allows for in situ or in operando visualization and tracking of solid phase formation.
• The high-throughput nature of SECCM-IRM facilitates large dataset generation for exploring experimental parameter landscapes.