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A key step in creating efficient and long-lasting catalysts is understanding their deactivation mechanism(s). On this basis, the behavior of a series of Pd/corundum materials during several hydrogen adsorption/desorption cycles was studied using temperature-programmed desorption coupled with mass spectrometry and aberration-corrected transmission electron microscopy. The materials, prepared by impregnation and by sputtering, presented uniform well-dispersed Pd nanoparticles. In addition, single atoms and small clusters of Pd were only detected in the materials prepared by impregnation. Upon exposure to hydrogen, the Pd nanoparticles smaller than 2 nm and the single atoms did not present any change, while the larger ones presented a core-shell morphology, where the core was Pd and the shell was PdH x . The results suggest that the long-term activity of the materials prepared by impregnation can be attributed solely to the presence of small clusters and single atoms of Pd., Competing Interests: The authors declare no competing financial interest., (© 2022 American Chemical Society.)

Several procedures were employed in the preparation of different Pd- and Fe-based catalytic membrane reactors (CMRs) via the normal wet impregnation method, reverse filtration of a microemulsion, sputtering method, and the precipitation of a Fe complex. Depending on the chosen procedure, the metal active phase can be found on the exterior and/or interior part of the CMR or even in its pores in concentrations between 0.05 and 2 wt %. Moreover, we have managed to implement a unique systematic process to grow hydrotalcite in the pores of a Pd-CMR. To exemplify the activity of these new CMRs, we have tested them in the peroxidation of phenol and in situ epoxidation of trans -chalcone., Competing Interests: The authors declare no competing financial interest., (Copyright © 2019 American Chemical Society.)