Skip to content

Electron Beam Transparent Boron Doped Diamond Electrodes for Combined Electrochemistry─Transmission Electron Microscopy

MetadataDetails
Publication Date2022-07-14
JournalACS Measurement Science Au
AuthorsHaytham E. M. Hussein, Georgia Wood, Daniel Houghton, Marc Walker, Yisong Han
InstitutionsUniversity of Warwick
Citations4

The majority of carbon based transmission electron microscopy (TEM) platforms (grids) have a significant sp<sup>2</sup> carbon component. Here, we report a top down fabrication technique for producing freestanding, robust, electron beam transparent and conductive sp<sup>3</sup> carbon substrates from boron doped diamond (BDD) using an ion milling/polishing process. X-ray photoelectron spectroscopy and electrochemical measurements reveal the sp<sup>3</sup> 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 <i>vs</i> 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, <i>in situ</i> 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.

  1. 2015 - Nanocharacterization