Co-ferrite was synthesized by HEBM (High Energy Ball Milling) with a stoichiometric (Co/Fe=0.5/2.5) mixture of CoO and $Fe_2O_3$ powders. The effect of milling time on the phase transformation of the mixture was investigated by XRD. Mono-phase solid solution of Co-ferrite, which was milled for 4 h and then calcined at $900^{circ}C$ in the Ar atmosphere, was confirmed by XRD analysis. The composition and thermal reduction behavior of Co-ferrite were analyzed by TGA and XRF. As a result, oxygen deficient Co-ferrite was synthesized by HEBM and the weight decrease of the Co-ferrite, which was oxidized at $600^{circ}C$ for 10h by $H_2O$ vapor, was 2.41 wt% during thermal reduction at $1300^{circ}C$.