To improve the ignition and combustion properties of n-Al powders, n-Al/Ni composite particles were prepared by replacement reaction under alkaline environment. In the anhydrous ethanol system, the effect of solution parameters on sample preparation was studied, and the preparation technology of n-Al/Ni was accordingly optimized. The chemical constituents, phase, morphology and combustion performances of n-Al/Ni were characterized by chemical titration, XRD, SEM, EDS and combustion duration test, respectively. The results showed that the optimized replacement reaction method can modify the n-Al powders by nickel well, and it was appropriate to use OH À 1 corresponding to consume 60 % alumina in the n-Al powders and Ni2 + equal to 12.35 % mass fraction of n-Al powders. It can be seen from the SEM images that the samples have a dispersive spherical morphology with a uniform distribution of nickel overall the samples. And the XRD results confirmed that nickel exists in the samples as a metallic substance. The results of chemical titration indicated that the content of active aluminum in the optimal sample was slightly higher than that of raw n-Al, but considering Ni, the content of reactive substance in the sample was greatly increased. The combustion duration test also proved that the combustion performance of n-Al/Ni was significantly improved. In conclusion, the improved properties promise a further enhanced prospect of n-Al in energetic materials.