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Title: Quantitative Electrochemical Measurements using in situ ec-S/TEM Devices

Insight into dynamic electrochemical processes can be obtained with in situ ec-S/TEM, which 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, choronoamperometry and electrochemical impedance spectroscopy were performed using a standard one electron transfer redox couple using a [Fe(CN)6]3-/4- based electrolyte. Established relationships of the electrode geometry and microfluidic conditions were fitted with cyclic voltammetry and chronoamperometic measurements of analyte diffusion coefficients and was found to agree with well-accepted values that are on the order of 10-5 cm2 s-1. 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.
 [1] ;  [1] ;  [1] ;  [1] ;  [1] ;  [1] ;  [2] ;  [2] ;  [2] ;  [2]
  1. ORNL
  2. Protochips Inc., Raleigh, NC
Publication Date:
OSTI Identifier:
DOE Contract Number:
Resource Type:
Journal Article
Resource Relation:
Journal Name: Microscopy and Microanalysis
Research Org:
Oak Ridge National Laboratory (ORNL); Center for Nanophase Materials Sciences (CNMS)
Sponsoring Org:
SC USDOE - Office of Science (SC)
Country of Publication:
United States