Fe-doped skutterudite with a nominal composition of has been synthesized by mechanical alloying (MA) of elemental powders, followed by hot pressing. Phase transformations during mechanical alloying and hot pressing were systematically investigated using XRD. Single phase skutterudite was successfully produced by vacuum hot pressing using as-milled powders without subsequent annealing. However, second phase in the form of marcasite structure was found to exist in case of , suggesting the solubility limit of Fe with Co in this system. Thermoelectric properties as functions of temperature and Fe contents were evaluated for the hot pressed specimens. Fe substitution up to x=1.5 with Co in appeared to increase thermoelectric figure of merit (ZT) and the maximum ZT was found to be 0.78 at 525K in this study.