A 90 wt% Mg-10 wt% NbF 5 sample was prepared by mechanical milling under H 2 (reactive mechanical grinding). Its hydriding and dehydriding properties were then examined. Activation of the 90 wt% Mg-10 wt% NbF 5 sample was not required. At n = 1, the sample absorbed 3.11 wt% H for 2.5 min, 3.55 wt% H for 5 min, 3.86 wt% H for 10 min, and 4.23 wt% H for 30 min at 593K under 12 bar H 2 . At n = 1, the sample desorbed 0.17 wt% H for 5 min, 0.74 wt% H for 10 min, 2.03 wt% H for 30 min, and 2.81 wt% H for 60 min at 593K under 1.0 bar H 2 . The XRD pattern of the 90 wt% Mg-10 wt% NbF 5 after reactive mechanical grinding showed Mg, β-MgH 2 and small amounts of γ-MgH 2 , NbH 2 , MgF 2 and NbF 3 . The XRD pattern of the 90 wt% Mg-10 wt% NbF 5 dehydrided at n = 3 revealed Mg, β-MgH 2 , a small amount of MgO and very small amounts of MgF 2 and NbH 2 . The 90 wt% Mg-10 wt% NbF 5 had a higher initial hydriding rate and a larger quantity of hydrogen absorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% Fe 2 O 3 , which were reported to have quite high hydriding rates and/or dehydriding rates. The 90 wt% Mg-10 wt% NbF 5 had a higher initial dehydriding rate (after an incubation period) and a larger quantity of hydrogen desorbed for 60 min than the 90 wt% Mg-10 wt% MnO and the 90 wt% Mg-10 wt% Fe 2 O 3 .