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Adsorption and thermal decomposition of Ni(CO)4 in the cage system of zeolite Y have been studied with EXAFS, electron microscopy and IR spectroscopy , Ni(CO)4 is adsorbed as an intact molecule in both cation - free zeolite Y and NaY. Symmetry changes of the molecule in NaY are assigned to the formation of Na—OC-IMi bridges. Thermal treatment of the Ni(CO)4/NaY adduct leads to loss of CO concomitant with the formation of a binodal Ni phase. A major part of the forms clusters with diameter between 0.5 and about 1.5 nm, in addition to larger crystallites (5-30 nm), sticking at the outer surface of the zeolite matrix., The Ni-Ni scattering amplitude indicates increasing average particle size with increasing temperature.