Abstract: The vacuum sintering process was selected to prepare NiAl₂O₃, and Fe powder was added to obtain excellent conductivity of the sample. The phase composition, microstructure, and electromagnetic properties of the alloy were tested by experiments. The results show that after increasing Fe content gradually, a stronger Fe diffraction peak is formed, and NiAl₂O₃ diffraction peak intensity decreases. Fe and NiAl₂O₃ form a good compatibility state, and NiAl₂O₃/Fe sample with excellent high-temperature stability is prepared. After increasing the amount of Fe, the porosity of the matrix microstructure decreases, which makes the alloy microstructure reach a more compact state. When a higher proportion of Fe is added, the sample shows a positive reactance value, showing obvious sensitivity resistance, and the positive reactance value and frequency show an increasing trend. The increase in frequency results in a significant increase in resistance and a decrease in conductivity. The NiAl₂O₃ alloy without Fe powder added does not show prominent magnetic properties. When Fe content is low, the sample obtains paramagnetism. After increasing the amount of Fe, the sample shows apparent dispersion. The sample with the Fe content of 40% forms an evident relaxation magnetic spectrum with diamagnetism and realizes the double negative property.