Journal article
In-situ SEM microchip setup for electrochemical experiments with water based solutions
Center for Electron Nanoscopy, Technical University of Denmark1
Department of Micro- and Nanotechnology, Technical University of Denmark2
Molecular Windows, Department of Micro- and Nanotechnology, Technical University of Denmark3
NanoChemistry, Department of Chemistry, Technical University of Denmark4
Studying electrochemical (EC) processes with electron microscopes offers the possibility of achieving much higher resolution imaging of nanoscale processes in real time than with optical microscopes. We have developed a vacuum sealed liquid sample electrochemical cell with electron transparent windows, microelectrodes and an electrochemical reference electrode.
The system, called the EC-SEM Cell, is used to study electrochemical reactions in liquid with a standard scanning electron microscope (SEM). The central component is a microfabricated chip with a thin (50nm) Si-rich silicon nitride (SiNx) window with lithographically defined platinum microelectrodes.
We show here the design principles of the EC-SEM system, its detailed construction and how it has been used to perform a range of EC experiments, two of which are presented here. It is shown that the EC-SEM Cell can survive extended in-situ EC experiments. Before the EC experiments we characterized the beam current being deposited in the liquid as this will affect the experiments.
The first EC experiment shows the influence of the electron-beam (e-beam) on a nickel solution by inducing electroless nickel deposition on the window when increasing the current density from the e-beam. The second experiment shows electrolysis in EC-SEM Cell, induced by the built-in electrodes.
Language: | English |
---|---|
Year: | 2013 |
Pages: | 63-69 |
ISSN: | 18792723 and 03043991 |
Types: | Journal article |
DOI: | 10.1016/j.ultramic.2013.03.002 |
ORCIDs: | Mølhave, K. |