Using an optical technique to measure hydrogen sorption kinetics the catalytic activity of the NiOx clusters is determined. The thus measured temperature dependence reveals an activation energy of 0.58 eV. The catalytic activity of NiOx clusters is studied as a function of the oxygen concentration. The surface properties are analyzed by Auger-electron spectroscopy. It appears that the catalytic hydrogen sorption originates from the dissociative chemisorption of hydrogen on O: Ni, which is strongly suppressed by the presence of oxides. © 2004 American Institute of Physics.