| Summary: | High hydro-active Al-3Ga-3In-3Sn alloys were prepared by coupling alloying and mechanical milling methods. NiCl<sub>2</sub> was added to the alloy during ball milling as the catalyst. XRD, SEM, and XAFS were used for the characterization of the hydro-active alloy. The hydrogen generation properties were systematically investigated in tap water at room temperature. The results show that the hydrogen generation rate is 11.02 L∙min<sup>−1</sup>∙g<sup>−1,</sup> and the conversion yield is 90.25% for the Al-3Ga-3In-3Sn-2NiCl<sub>2</sub> composite with a ball milling time of 2 h at room temperature in tap water. The hydrolysis reaction contains the expansion of the Al-based phase into a nano-sized layer and the further hydrolysis reaction of the layered Al phase with water. The activation mechanism was also investigated, and the activation of Al was attributed to the Al-Ni galvanic with the existing Cl<sup>−</sup>, which leads to a faster hydrolysis reaction rate for ball-milled powder with NiCl<sub>2</sub>.
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