Without any surfactant, antiferromagnetic Co 3 O 4 nanoparticles were synthesized successfully for the first time by means of an oxidation-reduction method with cobalt sulfate as starting material, which was oxidized to cobalt salt by NaNO 3 after alkalinizing with NaOH. Morphological, structural, spectroscopic and magnetic characterization of the product were done by SEM, TEM, XRD, and VSM, respectively. The average crystallite size (on the base of line profile fitting method), D and σ, is estimated as 30 ± 6 nm. Some anomalous magnetic properties and their enhanced effect have been observed in Co 3 O 4 antiferromagnetic nanocrystallites, including a bias field, coercivity, permanent magnetic moments and an open loop. These phenomena are attributed to the unidirectional anisotropy which is caused by the exchange coupling between AFM and FM layers, the existence of the spin glass like surface spins of Co 3 O 4 nanoparticles due to size effects and surface-area effect.© Versita Warsaw and Springer-Verlag Berlin Heidelberg.