26–30 Aug 2024
Europe/Berlin timezone

In Situ Photo-Electrochemical Investigation Using Surface X-ray Diffraction: From Ultra-High Vacuum to Solid/Eelectrolyte Interfaces

30 Aug 2024, 14:40
20m
Saal E

Saal E

Invited talk 5. Diffraction and scattering for operando investigations Mikrosymposium 5/2: Operando Investigations

Speaker

Axel Wilson (CNRS)

Description

A custom apparatus was developed at I07 Surface and Interface Diffraction beamline, Diamond Light Source (DLS) to perform operando measurements of solid/electrolyte interfaces under external potential and UV illumination using surface X-ray diffraction (SXRD).
Samples can be prepared under ultra-high vacuum (UHV) using standard methods in DLS Surface and Interface Laboratory. Pre-characterisation such as low energy electron diffraction, scanning tunnelling microscopy and X-ray photoelectron spectroscopy (LEED, STM, XPS) can be performed prior to transferring the sample under UHV to the Photo-ElectroChemical DrOplet Cell (PEC-DOC). The PEC-DOC is then transferred and mounted of I07’s EH1 diffractometer for SXRD structure determination under UHV. A custom liquid delivery device comprising a working and reference electrodes is then introduced in the chamber under controlled atmosphere. A droplet of electrolyte is contacted to the surface using an endoscope, also utilised to monitor the shape of the droplet during acquisition.
Using the PEC-DOC, the electrical double layer of the TiO2(110) interface with 0.1 M KCl(aq) has been elucidated. This represents an insight into the behaviour of the semiconductor in a neutral interface to define the structure of the electrical double layer present. The electrochemical capabilities of the PEC-DOC enabled cyclic voltammograms of the surface interface to be recorded. It also allowed a bias voltage to be applied for SXRD measurements, providing a tentative insight into the electrochemical desorption taking place as a result of applied positive potential.
This work was supported by the European Research Council Advanced Grant ENERGYSURF to GT, EPSRC (EP/L015862/1). AW has received funding from the European Union’s research and innovation programme under the Marie Sklodowska-Curie grant GA No 665593.

I plan to submit also conference proceedings Yes

Primary author

Axel Wilson (CNRS)

Co-authors

Dr Debi Garai (Diamond Light Source) Prof. Geoff Thornton (University College London) Dr Hadeel Hussain (Diamond Light Source) Dr Immad Nadeem (University College London) Mr Jameel Imran (University College London) Dr Jörg Zegenhagen (Diamond Light Source) Dr Xavier Torrelles (Institute of Materials Science of Barcelona)

Presentation materials