Abstract: Fe-TiCN composite powders were prepared via carbothermic reduction of milled titanium concentrate with ilmenite and graphite as raw materials. The effect of milling parameters on the titanium concentrate/ graphite mixed powders was studied with XRD, TG-DSC and SEM analysis. When the milling time was 4 h and the milling speed was 450 r/min, amorphous state of graphite would accelerate the reduction process. The onset reaction temperature was advanced by 360 ℃ and reached platform with a total loss of 35 %.