12.2 Two-Plate Thin-Layer Cells for Electron Microscopic …
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with very high doping level sandwiched between the electrode metal and a SiO 2
insulating layer [29]. This electrical contact is driven outside the cell for creating an
external electrical contact point. This connection made has a great advantage for a
multiple electrode arrangement.
The arrangement of the electrodes may vary depending on the goal of the experiment. Figure 12.5 offers a basic overview of the systems commonly found in the relevant literature. It is noteworthy that in situ synchrotron-based soft X-ray microscopy
Fig. 12.5 a Thin-layer TEM cell structure for nucleation studies where the electron beam is passed
through the surface of the working electrode. 1: bottom Si wafer (with high doping level for good
conductivity), 2: Si 3 N 4 layer on the bottom wafer (electrically insulating), 3: external contact for the
working electrode, 4: spacer layer with the thickness equivalent to the solution layer thickness above
the working electrode, 5: working electrode, Au, with ~20 nm thickness (there is no Si 3 N 4 layer
between the working electrode/external contact point and the Si wafer for providing the electrical
contact), 6: observation window with 30–80 nm thick Si 3 N 4 layer only at the bottom wafer, 7: top Si
wafer, 8: Si 3 N 4 observation window on the top part, 9: top chambers for counter/reference electrode
and/or for connectors to the solution flow system. Figure was sketched after [31–34]. b Example for
the electrode arrangement when the current direction is in the plane of the thin solution layer (top
view). Here, the electrodes can be a few tens of micrometre wide, several hundred nanometre thick
and are not transparent for the electron beam. The dashed line shows the Si 3 N 4 window. Figure was
sketched after [35]. c Photograph of a fully assembled in situ electrochemical TEM cell. The width
of the black end part can be between 6 and 15 mm for various devices. Figure 12.5c is reprinted
from Ref. [36]. Copyright (2012), with permission from Elsevier
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