Due to its large hydrogen capacity (10.1 wt.%), aluminium hydride (AlH₃) is considered as a possible material for on-board hydrogen storage applications. However, several factors, such as its high decomposition temperature and sluggish desorption kinetics, limit this benefit and render this material unmarketable. To overcome these limitations, numerous studies have been conducted, such as using mechanical milling to reduce the particle size and adding dopants or catalysts. In this work, the effect of metals (Ni and Fe) on the dehydrogenation properties of AlH₃ has been investigated for the first time. The results show that Ni is a better catalyst than Fe when it comes to lowering the initial decomposition temperature and speeding up the process of AlH₃ desorption. The 10 wt.% Ni-doped AlH₃ sample's starting decomposition temperature dropped from 130 °C to 80 °C compared to that of as-milled AlH₃. In the desorption kinetic measurements at 100 °C, the 10 wt% Ni-doped AlH₃ sample desorbed about 6.7 wt% of H₂ in 20 min compared to the 4.5 wt% desorption exhibited by the as-milled AlH₃. After Ni was added, the activation energy for the dehydrogenation process of AlH₃ that was determined by Kissinger analysis was decreased. From the X-ray diffraction analysis, we found that Ni did not react with AlH₃ during the mechanical milling and heating (desorption) processes. Ni is believed to play a catalytic role by inducing Ni-H interaction and weakening Al-H bonding, which improves the dehydrogenation storage properties of AlH₃.