Nanoscale electrochemical movies and synchronous topographical mapping of electrocatalytic materials

Faraday Discussions
Cameron L Bentley, Patrick R Unwin

Abstract

Techniques in the scanning electrochemical probe microscopy (SEPM) family have shown great promise for resolving nanoscale structure-function (e.g., catalytic activity) at complex (electro)chemical interfaces, which is a long-term aspiration in (electro)materials science. In this work, we explore how a simple meniscus imaging probe, based on an easily-fabricated, single-channeled nanopipette (inner diameter ≈ 30 nm) can be deployed in the scanning electrochemical cell microscopy (SECCM) platform as a fast, versatile and robust method for the direct, synchronous electrochemical/topographical imaging of electrocatalytic materials at the nanoscale. Topographical and voltammetric data are acquired synchronously at a spatial resolution of 50 nm to construct maps that resolve particular surface features on the sub-10 nm scale and create electrochemical activity movies composed of hundreds of potential-resolved images on the minutes timescale. Using the hydrogen evolution reaction (HER) at molybdenite (MoS2) as an exemplar system, the experimental parameters critical to achieving a robust scanning protocol (e.g., approach voltage, reference potential calibration) with high resolution (e.g., hopping distance) and optimal scan times (e....Continue Reading

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Oct 24, 2017·Journal of the American Chemical Society·Cameron L BentleyPatrick R Unwin

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Citations

Jan 4, 2020·Chemical Communications : Chem Comm·Yuying GaoCan Li
Jun 25, 2021·Chemical Science·N LimaniR Cornut
Dec 1, 2018·Analytical Chemistry·Cameron L BentleyPatrick R Unwin
Nov 30, 2018·Journal of the American Chemical Society·Cameron L BentleyPatrick R Unwin

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Methods Mentioned

BETA
electrochemical cell microscopy
scanning electron microscopy
Scanning Probe Microscopy
transmission electron microscopy
AFM

Software Mentioned

SPIP
SECCM
OriginPro
OriginLab
Matlab
LabVIEW

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