Abstract Ni x Cu 1−x Fe 2 O 4 nanocrystals were prepared by co-precipitation technique to study the electromagnetic (EM) wave absorption properties. The XRD and SEM results confirm the formation of single-phase cubic spinel structure and reveal that the crystallite size decreases with the addition of Ni content. The vibrating sample magnetometer results showed that the as-prepared material was soft magnetic and have potential applications in magnetic storage technology and field sensors. The dielectric parameters and EM wave absorption characteristics of Ni x Cu 1−x Fe 2 O 4 nanocrystals were studied in the frequency range of 1-18GHz using a vector network analyzer. The permittivity, impedance matching, and EM wave absorption of the materials are significantly improved with the increase in Ni content. The lowest value of reflection loss (R L ) is observed −22.8 dB at 16.09 GHz (R L ≤ −10dB, absorption >90%), showing an optimal EM wave absorption performance, which might generate from the synergistic effect between relative permittivity and permeability.