Abstract
It is well-known that synchrotron-based techniques are useful for the investigation of functional materials under working conditions. Some examples can be found in heterogeneous catalysis, as well as in thin film growth, specifically using atomic layer deposition. The presentation will focus on some examples, with a particular emphasis on the use of in situ and operando techniques in the context of dry reforming of methane (DRM), a reaction of environmental relevance that simultaneously valorises CH4 and CO2 into syngas, CoRu-based catalysts synthesized via mechanochemistry have demonstrated a synergy between cobalt and ruthenium that enhances reducibility, dispersion, and surface reactivity. In situ and operando techniques such as NAP-XPS, XRD, and XAS have provided information about surface dynamics, structural evolution and the local coordination environment during catalyst reduction and the DRM reaction.
Complementary studies in atomic layer deposition (ALD) have focused on the development of a home-built ALD reactor, which enables tracking the thin film growth using XAS and GISAXS, at ALBA synchrotron beamlines NOTOS and NCD-Sweet. Validation of the reactor was carried out by performing in situ XAS during TiO2 deposition, correlating edge-jump evolution with film thickness and phase formation. Additionally, GISAXS was used to characterize TiO2, as well as to monitor the infiltration of Al2O3 in block copolymer templates.
These studies highlight a common methodological framework: the in situ investigation of surface and interface phenomena under working conditions, enabling the rational design of advanced functional materials and processes.
InCAEM Project