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Electron beam transparent boron doped diamond electrodes for combined electrochemistry─transmission electron microscopy
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Hussein, Haytham E. M., Wood, Georgia F., Houghton, Daniel, Walker, Marc, Han, Yisong, Zhao, Pei, Beanland, Richard and Macpherson, Julie V. (2022) Electron beam transparent boron doped diamond electrodes for combined electrochemistry─transmission electron microscopy. ACS Measurement Science Au, 2 (5). pp. 439-448. doi:10.1021/acsmeasuresciau.2c00027 ISSN 2694-250X.
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WRAP-Electron-beam-transparent-boron-doped-diamond-electrodes-for-combined-electrochemistry-transmission-electron-microscopy-Houghton-2022.pdf - Published Version - Requires a PDF viewer. Available under License Creative Commons Attribution 4.0. Download (5Mb) | Preview |
Official URL: https://doi.org/10.1021/acsmeasuresciau.2c00027
Abstract
The majority of carbon based transmission electron microscopy (TEM) platforms (grids) have a significant sp2 carbon component. Here, we report a top down fabrication technique for producing freestanding, robust, electron beam transparent and conductive sp3 carbon substrates from boron doped diamond (BDD) using an ion milling/polishing process. X-ray photoelectron spectroscopy and electrochemical measurements reveal the sp3 carbon character and advantageous electrochemical properties of a BDD electrode are retained during the milling process. TEM diffraction studies show a dominant (110) crystallographic orientation. Compared with conventional carbon TEM films on metal supports, the BDD-TEM electrodes offer superior thermal, mechanical and electrochemical stability properties. For the latter, no carbon loss is observed over a wide electrochemical potential range (up to 1.80 V vs RHE) under prolonged testing times (5 h) in acid (comparable with accelerated stress testing protocols). This result also highlights the use of BDD as a corrosion free electrocatalyst TEM support for fundamental studies, and in practical energy conversion applications. High magnification TEM imaging demonstrates resolution of isolated, single atoms on the BDD-TEM electrode during electrodeposition, due to the low background electron scattering of the BDD surface. Given the high thermal conductivity and stability of the BDD-TEM electrodes, in situ monitoring of thermally induced morphological changes is also possible, shown here for the thermally induced crystallization of amorphous electrodeposited manganese oxide to the electrochemically active γ-phase.
Item Type: | Journal Article | |||||||||
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Subjects: | Q Science > QD Chemistry | |||||||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry Faculty of Science, Engineering and Medicine > Science > Physics |
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Library of Congress Subject Headings (LCSH): | Boron, Diamonds, Artificial, Transmission electron microscopy | |||||||||
Journal or Publication Title: | ACS Measurement Science Au | |||||||||
Publisher: | ACS | |||||||||
ISSN: | 2694-250X | |||||||||
Official Date: | 19 October 2022 | |||||||||
Dates: |
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Volume: | 2 | |||||||||
Number: | 5 | |||||||||
Page Range: | pp. 439-448 | |||||||||
DOI: | 10.1021/acsmeasuresciau.2c00027 | |||||||||
Status: | Peer Reviewed | |||||||||
Publication Status: | Published | |||||||||
Access rights to Published version: | Open Access (Creative Commons) | |||||||||
Date of first compliant deposit: | 28 March 2023 | |||||||||
Date of first compliant Open Access: | 29 March 2023 | |||||||||
RIOXX Funder/Project Grant: |
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