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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−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. [ABSTRACT FROM AUTHOR]