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Related Experiment Video

Updated: May 20, 2026

Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope (AFM-SECM)

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Published on: February 10, 2021

Resolving Microscale Selectivity of Electrochemical CO₂ Reduction Using Hybrid Dual-Probe Scanning Electrochemical

Moonjoo Kim¹, Lejing Li¹, Thomas Quast¹

¹Analytical Chemistry - Center for Electrochemical Sciences (CES), Faculty of Chemistry and Biochemistry, Ruhr University Bochum, Universitätsstraße 150, Bochum 44801, Germany.

|May 19, 2026

Summary

This study integrates scanning electrochemical cell microscopy (SECCM) with scanning electrochemical microscopy (SECM) to map the selectivity of the electrochemical carbon dioxide reduction reaction (CO2RR) at the nanoscale. This hybrid technique reveals microscale variations in catalyst performance, crucial for developing efficient CO2RR systems.

Keywords:

CO2 reduction SECM−SECCM nanoelectrochemistry scanning electrochemical cell microscopy (SECCM)scanning electrochemical microscopy (SECM)selectivity

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Published on: August 4, 2023

Area of Science:

Electrochemistry
Catalysis
Materials Science
Nanotechnology

Background:

The electrochemical carbon dioxide reduction reaction (CO2RR) is vital for converting CO2 into valuable products but suffers from competing hydrogen evolution and complex product selectivity.
Electrocatalysts for CO2RR exhibit spatial heterogeneity in activity and selectivity, making nanoscale investigation essential.
Existing scanning electrochemical cell microscopy (SECCM) techniques lack direct selectivity mapping capabilities for CO2RR.

Purpose of the Study:

To develop and demonstrate a hybrid SECCM-SECM platform for investigating local selectivity in CO2RR.
To elucidate the role of redox cycling and gas exchange at the three-phase boundary in CO2RR.
To map the microscale selectivity heterogeneity of Ag-Bi2O3 catalysts for CO2RR.

Main Methods:

Integration of SECCM with SECM, utilizing nanoelectrodes within the SECCM tip for high collection efficiency.
Employing substrate generation/tip collection (SG/TC) mode voltammetry during CO2RR on Au and Bi substrates.
Utilizing formate redox cycling to map local formate selectivity on Ag-Bi2O3 catalysts.

Main Results:

Achieved high collection efficiency (98.2 ± 2.1%) for redox cycling using SECCM-SECM with submicrometer tip-substrate separation.
Identified the critical roles of redox cycling and gas exchange at the three-phase boundary in governing local CO2RR product distribution (CO, formate, H2).
Successfully mapped the microscale heterogeneity in formate selectivity of Ag-Bi2O3 catalysts as a function of applied potential.

Conclusions:

The hybrid SECCM-SECM technique provides unprecedented nanoscale insights into CO2RR selectivity.
This method is powerful for understanding dynamic structure-activity-selectivity relationships in CO2RR electrocatalysis.
The findings pave the way for designing more efficient and selective electrocatalysts for CO2 conversion.