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27 results

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  • Overcoming the Challenges of Beam-sensitivity in Fuel Cell Electrodes
  • David A. Cullen, Brian T. Sneed, Karren L. More
  • Journal: Microscopy and Microanalysis / Volume 23 / Issue S1 / July 2017
  • Published online by Cambridge University Press: 04 August 2017, pp. 2222-2223
  • Print publication: July 2017
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  • Quantitative Electrochemical Measurements Using In Situ ec-S/TEM Devices
  • Raymond R. Unocic, Robert L. Sacci, Gilbert M. Brown, Gabriel M. Veith, Nancy J. Dudney, Karren L. More, Franklin S. Walden II, Daniel S. Gardiner, John Damiano, David P. Nackashi
  • Journal: Microscopy and Microanalysis / Volume 20 / Issue 2 / April 2014
  • Published online by Cambridge University Press: 11 March 2014, pp. 452-461
  • Print publication: April 2014
  • View abstract

    Insight into dynamic electrochemical processes can be obtained with in situ electrochemical-scanning/transmission electron microscopy (ec-S/TEM), a technique that utilizes microfluidic electrochemical cells to characterize electrochemical processes with S/TEM imaging, diffraction, or spectroscopy. The microfluidic electrochemical cell is composed of microfabricated devices with glassy carbon and platinum microband electrodes in a three-electrode cell configuration. To establish the validity of this method for quantitative in situ electrochemistry research, cyclic voltammetry (CV), choronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) were performed using a standard one electron transfer redox couple [Fe(CN)6]3−/4−-based electrolyte. Established relationships of the electrode geometry and microfluidic conditions were fitted with CV and chronoamperometic measurements of analyte diffusion coefficients and were found to agree with well-accepted values that are on the order of 10−5 cm2/s. Influence of the electron beam on electrochemical measurements was found to be negligible during CV scans where the current profile varied only within a few nA with the electron beam on and off, which is well within the hysteresis between multiple CV scans. The combination of experimental results provides a validation that quantitative electrochemistry experiments can be performed with these small-scale microfluidic electrochemical cells provided that accurate geometrical electrode configurations, diffusion boundary layers, and microfluidic conditions are accounted for.

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