The capability to perform liquid in situ transmission electron microscopy (TEM) experiments provides an unprecedented opportunity to examine the real-time processes of physical and chemical/electrochemical reactions during the interaction between metal surfaces and liquid environments. This work describes the requisite steps to make the technique fully analytical, from sample preparation, through modifications of the electrodes, characterization of electrolytes, and finally to electrochemical corrosion experiments comparing in situ TEM to conventional bulk cell and microcell configurations.
Using a hybrid sample preparation technique, FIB sections of electropolished stainless steel were welded to the platinum working electrode of an in-situ electrochemistry E-chip. Key elements of the design of the E-chip enabled a direct line of site to an EDS detector for elemental analysis and the working electrode was located off the window to facilitate attachment of the FIB section. The dissolution of a MnS inclusion was observed in situ an monitored with by EDS analysis. The corrosion potential of the sample was measured using a potentiodynamic polarization scan and the in-situ results agreed with bulk sample validating the use of LC-TEM electrochemical measurements for the study of bulk sample materials.