A Patterning Approach to Untangling Critical Interface Phenomena with <i>In-Situ</i> Resonant Scattering

Resonant soft x-ray scattering (RSoXS) is a powerful spatiochemical mesoscale characterization tool that is often overlooked across the field of interfacial science. Herein, we present a simple, yet highly sensitive, patterning approach for interface characterization that takes advantage of the physical processes intrinsic to small angle resonant X-ray scattering in order to selectively probe and enhance signals from interfacial regions of a vast array of material systems. Using several case studies, we show how patterns with simple nanoscale features can be used to 1) decouple the bulk from the interface scattering signal, 2) extract interfacial morphology with sub-nm precision, and 3) collect site-specific x-ray absorption spectra (XAS).
First, as an operando demonstration, we leverage a custom in-situ cell compatible with many synchrotron X-ray beamlines and use it conduct an operando study of Ni/Ni(OH)2 core/shell electrode undergoing electrochemical cycling under aqueous conditions. Next, we apply the technique to study the femtosecond dynamics of a 1.5 nm SiO2 surface with a broadband XUV table-top source. Finally, we introduce the potential of this technique to study material interfaces under conditions critical to the future of the next generation of electronics.