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Prabu, Vinod ; Obst, Martin ; Hosseinkhannazer, Hooman ; Reynolds, Matthew ; Rosendahl, Scott ; Wang, Jian ; Hitchcock, Adam P.:
Instrumentation for in-situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM).
In: Review of Scientific Instruments.
Bd. 89
(2018)
Heft 6
.
- No. 063702.
ISSN 1089-7623
DOI: https://doi.org/10.1063/1.5023288
Abstract
We report the design and performance of a 3-electrode device for real time in-situ Scanning Transmission X-ray Microscopy (STXM) studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolyte. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential & time of the spatial distributions of Cu(0) and Cu(I) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for reduction of Cu(II).