4.6 Article

A nanoporous diamond particle microelectrode and its surface modification

Journal

ELECTROCHIMICA ACTA
Volume 430, Issue -, Pages -

Publisher

PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.electacta.2022.141015

Keywords

Nanoporous interface; Thermal catalytic etching; Boron -doped diamond; Particle microelectrode; Surface modification

Funding

  1. National Key Research and Development Program of China [2021YFB3701803, 2016YFB0301400]
  2. National Natural Science Foundation of China [52071345, 51874370]
  3. Province Key Research and Development Program of Guang- dong [2020B010185001]

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This study presents a method to fabricate a single nanoporous diamond particle microelectrode with improved electrocatalytic performance. The modified nanoporous microelectrode exhibited a higher electron transfer kinetic constant and improved electrical conductivity.
Boron doped diamond electrode (BDDE) with dimensions of tens of or hundreds of mu m has received widespread attention for electrochemical and biological applications because of exceptional features such as wide potential window for water stability, excellent electrochemical/chemical stability, and superior antifouling properties. This work reported a feasible way to fabricate a single nanoporous BDD particle microelectrode (sDPME) using a commercial single-crystal BDD particle (cBDD) as the substrate. The nanoporous surface of cBDD (pcBDD) was formed via thermal catalytic treatment with nickel as the catalyst, followed by further electrodeposition of gold nanoparticles (Au NPs) to fill the nanopores, increasing its electrocatalytic performance. As a comparison, the heavily-doped polycrystalline BDD film was deposited on cBDD via hot-filament chemical vapor deposition, increasing its electrical surface conductivity, followed by the similar thermal etching to form the nanoporous surface (prBDD) as well as Au NPs modification. We gradually characterized surface modification of cBDD using scanning electron microscopy, Raman, energy dispersive spectroscopy and various electrochemical techniques. The results demonstrated that among six sDPMEs, the Au NPs-modified nanoporous sDPMEs (Au/prBDD) have one order of magnitude higher heterogeneous electron transfer kinetic constant than the cBDD. This difference was attributed to synergistic effects of the improved electrical conductivity (with a higher doping level of few 1020 cm-3 versus 1018 cm-3), the improved capability for electron transfer (with lower charge transfer resistance of 1.3 k ohm versus 8.6 k ohm) as well as the increased electrochemically active surface area (1.12 mm2 versus 0.34 mm2).

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