Al–Bi–Sn–Cu composite powders for hydrogen generation were designed from the calculated phase diagram and prepared by the gas atomization process. The morphologies and structures of the composite powders were investigated using X-ray diffraction (XRD) and a scanning electron microscope (SEM) equipped with energy-dispersive X-ray (EDX) spectroscopy, and the results indicate that the Cu additive enhanced the phase separation between the Al-rich phase and the (Bi, Sn)-rich phase. The hydrogen generation performances were investigated by reacting the materials with distilled water. The Al–Bi–Sn–Cu powders reveal a stable hydrogen generation rate, and the Al–10Bi–7Sn–3Cu (wt%) powder exhibits the best hydrogen generation performance in 50 °C distilled water which reaches 856 mL/g in 800 min. In addition, the antioxidation properties of the powders were also studied. The Al–10Bi–7Sn–3Cu (wt%) powder has a good resistance to oxidation and moisture, which shows great potential for being the hydrogen source for fuel cell applications.

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