Photocatalytic setup for in situ and operando ambient-pressure X-ray photoelectron spectroscopy at MAX IV Laboratory

Abstract

The Ambient-Pressure X-ray Photoelectron Spectroscopy (APXPS) endstation at the SPECIES beamline at MAX IV Laboratory has been improved. The latest upgrades help in performing photo-assisted experiments under operando conditions in the mbar pressure range using gas and vapour mixtures whilst also reducing beam damage to the sample caused by X-ray irradiation. This article reports on endstation upgrades for APXPS and examples of scientific cases of in situ photocatalysis, photoreduction and photo-assisted atomic layer deposition (photo-ALD).

Solar light driven atomic and electronic transformations in a plasmonic Ni@NiO/NiCO3 photocatalyst revealed by ambient pressure X-ray photoelectron spectroscopy

“… 32 When the solar simulator was turned ON, an increase in C 1s intensity at 285 eV was observed, corresponding to adventitious carbon. Since the solar simulator emits also IR radiation, 26 the catalyst surface becomes heated and the sample temperature can reach up to a maximum of 90 °C according to the thermocouple reading on the sample plate. Under UHV, with light illumination, adventitious carbon accumulated on the catalyst surface most probably due to the high catalyst surface temperatures.…”

“…24,25 As a part of in situ photocatalysis experiments, a solar simulator (Asahi HAL-320) was installed at the APXPS endstation. 26 The solar simulator was equipped with an AM 1.5 filter, which allows light to pass through in spectral ranges between 350 and 1100 nanometers. The light from the solar simulator is directed at the sample through a fused silica viewport on the UHV chamber and passes through a sapphire window on the ambient pressure cell.…”

“…The schematic layout of this setup and the solar simulator spectra recorded with both windows are shown elsewhere. 26 The photocatalyst used in this work is commercially available Ni nanoparticles from Hongwu International. Due to possible oxidation and carbonation while the metal nanoparticles are mass produced, these Ni nanoparticles are transformed into a complex Ni@NiO/NiCO 3 core@shell morphology.…”

“…The schematic layout of this setup and the solar simulator spectra recorded with both windows are shown elsewhere. 26 …”