The reasons for changes in catalytic activity as a function of the time of mechanochemical activation in a planetary mill were studied with the use of a set of physicochemical techniques. The dependence of the specific rate of CO oxidation on the time of mechanochemical activation exhibited an extremal character. Small-angle interblock boundaries, disordered dislocations, and shear defects were formed in the sample with maximum activity because of mechanochemical activation. The linear dependence of the specific rate of CO oxidation on the value of microstresses suggested that the above defects were responsible for an increase in the catalytic activity. It is likely that oxygen atoms situated at the sites of the outcrop of defects on the surface served as elementary active centers.