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Nanoscale electrochemical movies and synchronous topographical mapping of electrocatalytic materials
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Bentley, Cameron Luke and Unwin, Patrick R. (2018) Nanoscale electrochemical movies and synchronous topographical mapping of electrocatalytic materials. Faraday Discussions, 210 . 365-379 . doi:10.1039/c8fd00028j ISSN 0301-7249.
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Official URL: https://doi.org/10.1039/c8fd00028j
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.g., voltammetric scan rate, approach rate etc.) are considered and discussed. Furthermore, sub-nanoentity reactivity mapping is demonstrated with glassy carbon (GC) supported single-crystalline {111}-oriented two-dimensional Au nanocrystals (AuNCs), which exhibit uniform catalytic activity at the single-entity and sub-single entity level. The approach outlined herein signposts a future in (electro)materials science in which the activity of electroactive nanomaterials can be viewed directly and related to structure through electrochemical movies, revealing active sites unambiguously.
Item Type: | Journal Article | |||||||||
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Subjects: | Q Science > QD Chemistry Q Science > QH Natural history |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | |||||||||
SWORD Depositor: | Library Publications Router | |||||||||
Library of Congress Subject Headings (LCSH): | Scanning electrochemical microscopy, Electrocatalysis, Meniscectomy, Nanochemistry | |||||||||
Journal or Publication Title: | Faraday Discussions | |||||||||
Publisher: | Royal Society of Chemistry | |||||||||
ISSN: | 0301-7249 | |||||||||
Official Date: | 1 October 2018 | |||||||||
Dates: |
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Volume: | 210 | |||||||||
Page Range: | 365-379 | |||||||||
DOI: | 10.1039/c8fd00028j | |||||||||
Status: | Peer Reviewed | |||||||||
Publication Status: | Published | |||||||||
Access rights to Published version: | Restricted or Subscription Access | |||||||||
Date of first compliant deposit: | 5 October 2018 | |||||||||
Date of first compliant Open Access: | 22 March 2019 | |||||||||
RIOXX Funder/Project Grant: |
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