1. Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)
- Author
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Hooman Hosseinkhannazer, Jian Wang, Vinod Prabu, Martin Obst, Scott M. Rosendahl, Adam P. Hitchcock, and Matthew Reynolds
- Subjects
Working electrode ,Materials science ,Silicon ,Analytical chemistry ,chemistry.chemical_element ,02 engineering and technology ,Scanning transmission X-ray microscopy ,010402 general chemistry ,021001 nanoscience & nanotechnology ,Electrochemistry ,01 natural sciences ,Copper ,0104 chemical sciences ,chemistry ,Microscopy ,0210 nano-technology ,Absorption (electromagnetic radiation) ,Instrumentation ,Microfabrication - Abstract
We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. 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 and 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 the reduction of Cu(ii).
- Published
- 2018