Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

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).

Ice nucleation imaged with X-ray spectro-microscopy

“…The INXCell is advantageous for future studies of, e.g. phase transitions, chemical reactions, or multiphase chemistry, but potentially in other disciplines such as electrochemistry 106 for fuel cell performance, 126,127 involving the aqueous phase of liquid water where water saturation is maintained for long time scales.…”

Advanced Characterization in Clean Water Technologies

“…We note that STXM, although it employs relatively low energies, does not require UHV; typically, experiments are run in 0.2 atm He, implying that in situ experiments are possible. 34 Finally, we note that STXM can be performed ex situ in three dimensions. 35 X-ray fluorescence (XRF) imaging is another method that provides spatially resolved chemical information based on XAS.…”

In-Situ High-Temperature Heating Setup for Spectronanoscopy at Pohang Light Source

“…For in-situ heating transmission electron microscopy (TEM), previous use of a specimen holder with an attached filament heater caused problems [3]. There have been improvements that have made performing in-situ heating easier such as the development of microelectromechanical system (MEMS)-based heating microchips [4,5]. MEMS-based chips enable researchers to conduct thermal studies in a controlled and stable environment, even at 1000 ∘ C [6,7].…”