Soft X-ray Induced Radiation Damage in Dip-and-Pull Photon Absorption and Photoelectron Emission Experiments

X-ray irradiation can induce chemical reactions on surfaces. In X-ray spectroscopic experiments, such reactions may result in spectrum distortion and are termed radiation damage. In this study, we investigate the X-ray-induced chemical reaction at the partially oxidized copper surface in the settings of the dip-and-pull experiment, a method that generates liquid–solid interfaces for in situ X-ray photoelectron spectroscopy (XPS) studies. In dense water vapor resembling the predipping condition, a series of time-elapsed X-ray absorption spectra acquired in total electron yield mode (TEY-XAS) shows that X-ray exposure causes copper reduction, which follows first-order kinetics and occurs only at the surface shallower than the probing depth of TEY-XAS. At the solid–water interface created by the dip-and-pull method, the chemical reduction of surface copper is also identified by XPS. We conclude that the reduction is driven by the product of water radiolysis, where the reducing solvated electron prevails against the oxidizing OH radical and results in an overall reduction of surface copper ions.