Abstract: In the present contribution, some recent results by the author in the field of structural studies of catalysts are surveyed. Most experimental data were obtained at several beamlines of the Kurchatov Synchrotron Radiation Source (NRC “Kurchatov Institute”, Moscow). The techniques discussed include single-crystal and powder X-ray diffraction, X-ray Absorption Spectroscopy XANES/EXAFS, Small-Angle X-ray Scattering, etc. Some examples concern cage polynuclear metal-containing organosiloxanolates manifesting a pronounced catalytic activity in homogeneous oxidation, which is demonstrated by X-ray crystallographic identification of products of spontaneous and completely unexpected mild oxidation of ligands or solvents under synthesis conditions, including conversions of alcohol into carboxylate, THF into butyrolactone, phosphine into phosphine oxide, aromatic methyl of neocuproine into geminal diol. Another series of examples include structural monitoring of formation of catalytically active bimetallic nanoparticles from mixed-acetate molecular precursors (Pd-Zn, Pd-Ni, Pd-Eu, Pd-In, Pd-Pt, etc.). X-ray diffraction and XAFS implemented in situ make it possible to identify the sequence of distinct stages of the overall process initiated at different temperatures, such as chemical reduction of palladium, onset of reduction of the second metal, disordered solid solution emergence, intermetallic ordering, thermally activated growth of nanoparticles, etc. This knowledge enables fine control over the formation of nanoparticles to tailor their catalytic properties. As the final part of the talk, a brief introduction into new capabilities for the advanced diagnostics of catalysts imposed by the SKIF (Siberian Circular Photon Source), which is a project of a 4th-generation synchrotron centre near Novosibirsk being jointly developed by the Boreskov Institute of Catalysis and Budker Institute of Nuclear Physics, will be given. Acknowledgement. This work was supported by Ministry of Science and Higher Education of the Russian Federation (project АААА-А19-119020890025-3).

Cite: Zubavichus Y.V.
Structural Diagnostics of Catalysts Using X-Ray Synchrotron Radiation: Current Possibilities and Future Prospects
Bridging the Gap between Model and Real Catalysis. Synchrotron radiation in catalysis : 5th Russian-German Seminar on Catalysis 23-26 Jun 2019