Understanding Fe deposition in fluid catalytic cracking (FCC) catalysis is critical for the mitigation of catalyst degradation. Here we employ soft X-ray ptychography to determine at the nanoscale the distribution and chemical state of Fe in an aged FCC catalyst particle. We show that both particle swelling due to colloidal Fe deposition and Fe penetration into the matrix as a result of precracking of large organic molecules occur. The application of ptychography allowed us to provide direct visual evidence for these two distinct Fe-based deactivation mechanisms, which have so far been proposed only on the basis of indirect evidence.

Highly active catalysts for the oxygen evolution reaction (OER) are required for the development of photoelectrochemical devices that generate hydrogen efficiently from water using solar energy. Here, we identify the origin of a 500-fold OER activity enhancement that can be achieved with mixed (Ni,Fe)oxyhydroxides (Ni(1-x)Fe(x)OOH) over their pure Ni and Fe parent compounds, resulting in one of the most active currently known OER catalysts in alkaline electrolyte. Operando X-ray absorption spectroscopy (XAS) using high energy resolution fluorescence detection (HERFD) reveals that Fe(3+) in Ni(1-x)Fe(x)OOH occupies octahedral sites with unusually short Fe-O bond distances, induced by edge-sharing with surrounding [NiO6] octahedra. Using computational methods, we establish that this structural motif results in near optimal adsorption energies of OER intermediates and low overpotentials at Fe sites. By contrast, Ni sites in Ni(1-x)Fe(x)OOH are not active sites for the oxidation of water.