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Electron-beam deposited amorphous carbon films offer excellent conductivity and flatness for electrochemical applications. Protecting the surface with KCl enhances electron-transfer rate constants, crucial for accurate electrochemical measurements.

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Area of Science:

  • Electrochemistry
  • Materials Science
  • Surface Science

Background:

  • Amorphous carbon films produced by electron-beam deposition exhibit desirable properties for electrochemistry.
  • These films possess a flat surface (0.43 nm RMS roughness) and a mix of sp2/sp3 hybridization, ensuring conductivity.
  • The carbon films are suitable for optical spectroscopy due to their transparency and low background current.

Purpose of the Study:

  • To evaluate the performance of electron-beam deposited carbon (eC) electrodes for electrochemical measurements.
  • To investigate the impact of KCl protection on electron-transfer kinetics.
  • To demonstrate the utility of nanogap voltammetry for precise measurement of rate constants.

Main Methods:

  • Fabrication of ultra-flat amorphous carbon films via electron-beam deposition on gold substrates.
  • Protection of the carbon surface with a KCl layer deposited by e-beam under vacuum.
  • Utilizing nanogap voltammetry with scanning electrochemical microscopy (SECM) for electrochemical measurements.

Main Results:

  • The ultra-flat eC surface enabled nanogap voltammetry with small electrode-to-substrate gaps (44 nm), increasing the diffusion limit to >14 cm/s.
  • KCl-protected eC electrodes showed significantly enhanced heterogeneous standard electron-transfer rate constants (k°) for both ferrocene trimethylammonium and Ru(NH3)63+/2+.
  • For Ru(NH3)63+/2+, k° increased from 1.7 cm/s for unprotected eC to above 6.9 cm/s for KCl-protected eC.

Conclusions:

  • Electron-beam deposited amorphous carbon is a promising electrode material for electrochemistry due to its flatness and conductivity.
  • KCl surface protection effectively enhances electron-transfer kinetics, enabling more accurate measurements of rate constants.
  • Nanogap voltammetry on these protected electrodes provides a robust method for quantifying fast electron-transfer processes.