Abstract Lump-free Ni-5 wt% Al alloy powder was successfully prepared using an AlCl 3 activator at 400 °C under vacuum. The AlCl 3 activator served as the catalyst, lowering the fabrication temperature by 1000 °C compared with the temperature required for the conventional process. The Ni–Al alloy was formed by the following steps: the formation of NiAl by the reaction of the Ni surface with AlCl 2 or AlCl produced by the reaction between Al and AlCl 3 , the formation of Ni 3 Al by Al diffusion and reaction, and the formation of a Ni–Al solid solution by Al diffusion into the Ni matrix until the solubility limitation was reached. Although lowering the alloying temperature lengthens the reaction time, the time could be reduced by controlling the amount of AlCl 3 . A single cell test and a creep test were also conducted using a green sheet of as-prepared Ni–Al alloy powder as an anode of a molten carbonate fuel cell (MCFC).