Fe10Ag90 granular alloys have been prepared using a sol-gel process, sintered at 300 °C and annealed at temperatures between 400 °C and 700 °C. The mean size of the iron particles, obtained from X-ray diffraction, is 30.0 ± 0.7 nm. Due to the existence of a distribution of particle sizes in these samples, both blocked (BL) and superparamagnetic (SPM) particles are present simultaneously, as confirmed by magnetization measurements at room temperature. AC susceptibility measurements as a function of temperature reveal a magnetic phase transition at about 770 °C, indicating the presence of particles exhibiting bulk behavior, in the samples annealed above 550 °C. The presence of these particles has been attributed to an atomic diffusion process between the grains, forming bulk-like multiple-domain Fe particles having Curie temperatures near that of bulk alpha-Fe phase (T C = 770 °C).