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Mg-based metal hydrides are promising as hydrogen storage materials for fuel cell application. In this work, Mg2 FeH6 complex hydride phase was synthesized by controlled reactive ball milling of 2Mg-Fe (atomic ratio)powder mixture in H2. Mg2 FeH6 is confirmed to be formed via the following three stages: formation of MgH2 via the reaction of Mg with H2, incubation stage and formation of Mg2 FeH6 by reaction of fully refined MgH2 and Fe.The incubation stage is characterized by no traces of Mg or hydride crystalline phase by XRD. On the other hand,Mg is observed uniformly distributed in the milled powder by SEM-EDS. Also, almost the same amount of H2 as the first stage is detected stored in the powders of the second stage by DSC and TGA.