In an effort to synthesize homogenized single phase d-CoSb3, this study considers the mechanical alloying (MA) of elemental Co and Sb powders using a nominal stoichiometric composition followed by hot pressing. Single phase, undoped CoSb3 skutterudites were successfully produced by vacuum hot pressing using MA powders without subsequent annealing. Phase transformations during mechanical alloying, powder annealing, and hot pressing were systematically investigated using XRD and SEM. Thermoelectric properties were measured and compared with the results of similar studies. Temperature dependences were also evaluated, and their correlations to phase transformation were examined.