Published August 19, 2021 | Version v1
Journal article Open

Calibrating SECCM measurements by means of a nanoelectrode ruler. The intrinsic oxygen reduction activity of PtNi catalyst nanoparticles

  • 1. Analytical Chemistry–Center for Electrochemical Sciences, Faculty of Chemistry and Biochemistry, Ruhr University Bochum, Universitätsstr. 150, D-44780 Bochum, Germany
  • 2. Chemical Technology III, Faculty of Chemistry and CENIDE-Center for Nanointegration, University Duisburg Essen, Carl Benz Str. 199, D-47057 Duisburg, Germany
  • 3. School of Chemistry and Australian Centre for NanoMedicine, University of New South Wales, Sydney 2052, Australia
  • 4. Research Group of Functional Materials for Electrochemical Energy Conversion, School of Chemical Engineering, University of Science and Technology Liaoning, 114051 Anshan, China

Description

Scanning electrochemical cell microscopy (SECCM) is increasingly applied to determine the intrinsic catalytic activity of single electrocatalyst particle. This is especially feasible if the catalyst nanoparticles are large enough that they can be found and counted in post-SECCM scanning electron microscopy images. Evidently, this becomes impossible for very small nanoparticles and hence, a catalytic current measured in one landing zone of the SECCM droplet cannot be correlated to the exact number of catalyst particles. We show, that by introducing a ruler method employing a carbon nanoelectrode decorated with a countable number of the same catalyst particles from which the catalytic activity can be determined, the activity determined using SECCM from many spots can be converted in the intrinsic catalytic activity of a certain number of catalyst nanoparticles.

Notes

This project has received funding from the European Research Council (ERC) under the European Union's Horizon 2020 research and innovation programme (grant agreement CasCat [833408]) as well as from the European Union's Horizon 2020 research and innovation program under the Marie Skłodowska-Curie MSCA-ITN Single-Entity Nanoelectrochemistry, Sentinel [812398]. S. S. and C. A. acknowledge the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) within the project [440951282]. X. X. C. acknowledges financial support from the Liaoning BaiQianWan Talents Program, China (No. 2019B042), and the Excellent Young Scientific and Technological Talents Project of Educational Department of Liaoning Province, China (No. 2020LNQN07). We acknowledge Prof. Patrick Unwin from the University of Warwick for providing the initial control software (WEC-SPM) for our SECCM experiments.

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DOI10.1007s12274-021-3702-7.pdf

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Funding

SENTINEL – Single-Entity NanoElectrochemistry 812398
European Commission
CASCAT – Catalytic cascade reactions. From fundamentals of nanozymes to applications based on gas-diffusion electrodes 833408
European Commission