Single nanocrystalline spinel phases have been formed in mechanically alloyed CoFe 2O 4 and Co 0.8Fe 2.2O 4 powders after heat treatment at temperatures above 750°C. High coercivities (2.6–2.7kOe) were associated with nanocrystalline structures in CoFe 2O 4. In Co 0.8Fe 2.2O 4 a high remanence equal to 78% of the saturation magnetisation and a coercivity of 3.2kOe were obtained in magnetically annealed samples.