Dimagnesium iron hydride was synthesized by mechanical milling of a MgH2/Fe mixture followed by sintering under a high hydrogen pressure (120 bar). The influence of the milling time on the synthesis yield was observed. Properly chosen processing parameters led to a 94-97 % reaction yield (depending on the measurement method) for the formation of Mg2FeH6. Milling times that were too short or too long proved to be ineffective. A custom-made reactor for synthesis of a batch of up to 20 g is presented. Synthesized samples were characterized by XRD analysis and PCT measurements were performed. Copyright (C) 2012, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.