We reported on the hydrogen desorption properties, microstructure, kinetics, and decreased, compared with that of the sample ball-milled for 0.02 h. TEM observations revealed that the distribution of Nb 2 O 5 in MgH 2 was gradually improved during ball-milling. On the other hand, we confirmed by XPS that in the sample ball-milled for 0.2 h, Nb 2 O 5-x phase(s) existed at least on the surface. It can be suggested that these deoxidized Nb 2 O 5-x phases eventually decrease E a as substantial catalyst rather than Nb 2 O 5 itself.