|Prabu, V; Obst, M; Hosseinkhannazer, H; Reynolds, M; Rosendahl, S; Wang, J; Hitchcock, AP: Instrumentation for in-situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM), Review of Scientific Instruments (2018)|
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).
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