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In situ studies on reduction processes in praseodymium-doped ceria and nickel-loaded doped ceria nanoparticles have been investigated using environmental transmission electron microscopy. The presence of pit-like defects on the oxide nanoparticles resulted in amorphization during reduction. Hydrogen-spillover in nickel-loaded praseodymium-doped ceria (PDC) was directly observed. Localized reduction of ceria in a H 2 atmosphere was observed and attributed to gas–nickel–ceria interactions at the three-phase boundary. The spatial extent of the localized reduction zones was experimentally determined. The spillover mechanism is discussed in terms of surface diffusion properties of atomic hydrogen and oxygen species.