ACS Meas Sci Au
Department of Chemistry, University of Warwick, Coventry CV4 7AL, U.K.
Published: October 2022
The majority of carbon based transmission electron microscopy (TEM) platforms (grids) have a significant sp carbon component. Here, we report a top down fabrication technique for producing freestanding, robust, electron beam transparent and conductive sp carbon substrates from boron doped diamond (BDD) using an ion milling/polishing process. X-ray photoelectron spectroscopy and electrochemical measurements reveal the sp 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 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, 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.
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http://www.ncbi.nlm.nih.gov/pmc/articles/PMC9585633 | PMC |
http://dx.doi.org/10.1021/acsmeasuresciau.2c00027 | DOI Listing |
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