High coercivity nanostructured YCo5 powders were successfully prepared by mechanical milling of as-cast alloys and subsequent vacuum annealing. Almost single phase YCo5 alloys, obtained by arc melting, were processed by high energy mechanical milling using a SPEX 8000 mill. After 4 h of milling, powders become nearly amorphous. DSC scans revealed the existence of an irreversible broad exothermic transition with a maximum at 516 °C associated with the crystallization process. Annealing in high vacuum at 800 °C during 2.5 min led to the formation of YCo5 nanoparticles with an average particle size of 12 nm. A high intrinsic coercivity of 7.23 kOe together with a σr/σs ratio of 0.75 were obtained.