Electrochemical Measurements in In Situ TEM Experiments

Abstract

Potential sources of measurement error in electroanalytical analyses performed in-situ within a transmission electron microscope (TEM) are reported. Some relevant aspects of experimental set-up that impact noise are identified. The possibility of ground loops and recommendations that minimize them are presented. Offsets in the measured open circuit potential of working electrodes caused by the presence of the electron beam in TEM are demonstrated and discussed. This work also highlights the possibility of erroneous potential measurements when the electrode area exposed to electrolyte is significantly larger than the beam illumination area. General design criteria are proposed to assist in future electrochemical cell designs to mitigate electrochemical measurement artifacts inside a TEM.