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In this work, the NiCu solid solutions with different Ni/Cu molar ratios were prepared and then doped into MgH₂ through ball milling to modify its hydrogen sorption properties. The experimental results show that the Ni–25%Cu and Ni–50%Cu exhibit the superior catalytic effect over pure Ni, pure Cu and Ni–75%Cu on the dehydrogenation of MgH₂. Among them, the 5h-milled MgH₂/Ni–50%Cu system starts to desorb hydrogen at 205.8 °C, which is about 96.9 °C lower than that of as-milled pristine MgH₂. Moreover, the MgH₂/Ni-50% Cu system can release 5.14 wt% hydrogen at 300 °C within 15 min, while MgH₂ can only release 2.92 wt% hydrogen under the same condition. More importantly, the dehydrogenated MgH₂/Ni–50%Cu can reabsorb 4.37 wt% hydrogen even at 250 °C for 30 min. The enhanced hydrogen sorption kinetics of MgH₂/Ni–50%Cu mainly attributes to the “hydrogen spillover” effect of in-situ …