RT journal article T1 Understanding the evolution of ternary alloyed nanoparticles during reversible exsolution from double perovskite oxides A1 López García, Andrés A1 Carrillo, Alfonso J. A1 Jiménez, Catalina Elena A1 Suarez Anzorena, Rosario A1 García Diez, Raúl A1 Pérez Dieste, Virginia A1 Villar García, Ignacio J. A1 Hungría Hernández, Ana Belén A1 Bár, Marcus A1 Serra, José M. A2 Ciencia de los Materiales e Ingeniería Metalúrgica y Química Inorgánica AB Multicomponent nanoparticle exsolution has emerged as a promising process for obtaining highly active catalysts supported on perovskite oxides. For instance, FeCoNi alloys can be exsolved from Sr2FeCo0.2Ni0.2Mn0.1Mo0.5O6−d, boosting the electrocatalytic properties of these electrodes. However, due to differences incationdiffusion properties, the composition of the nanoparticles is uneven and strongly affected by process conditions such as temperature. An additional key feature of exsolution is its reversibility, which could help in catalyst regeneration if poisoned. Nevertheless, there is little knowledge on the reversibility mechanisms of multicomponent exsolved alloys. For that purpose, a combination of synchrotron-based in situ X-ray Diffraction (XRD) and Near-Ambient Pressure X-ray Photoelectron Spectroscopy (NAP-XPS) was employed in this work to uncover these missing aspects of multicomponent alloyed exsolution. These techniques allowed determination of the crystallographic and surface-related phenomena occurring during reversible exsolution both to the nanoparticles and the perovskite oxide support. This enabled the identification of the exsolution onset temperature and the range at which the double perovskite to Ruddlesden–Popper transition occurred, a process that has notable implications for the electrocatalytic performance. Finally, in combination with microscopy analyses, it was possible to reveal the morphological and compositional changes that the exsolvednanoparticlesexperiencedupon reductionoxidation cycles. This resulted in a re-arrangement of the surface species and a variation in the composition (Fe enrichment) of the regenerated ternary alloyed exsolved nanoparticles. These results indicate that reversible exsolution might alter the catalytic properties of the exsolved nanoparticles, with profound implications in the performance of (electro)catalytic processes. PB Royal Society of Chemistry SN 2050-7496 YR 2024 FD 2024 LK http://hdl.handle.net/10498/35876 UL http://hdl.handle.net/10498/35876 LA eng DS Repositorio Institucional de la Universidad de Cádiz RD 13-nov-2026