Abstract:The influences of the processing parameters on the Mg 2 FeH 6 synthesis yield were studied. Mixtures of magnesium hydride (MgH 2 ) and iron (Fe) were mechanically milled in a planetary ball mill under argon for 0.5-, 1-, 2-and 3-h periods and subsequently sintered at temperatures from 300-500 • C under hydrogen. The reaction yield, phase content and hydrogen storage properties of the received materials were investigated. The morphologies of the powders after synthesis were studied by SEM. The synthesis effectiveness map was presented. The obtained results prove that synthesis parameters, such as the milling time and synthesis temperature, greatly influence the reaction yield and material properties and show that extended mechanical milling may not be beneficial to the reaction efficiency.