The aim of the present study is to employ the mechanical alloying method to develop a composite material comprising of nickel ferrite and activated carbon. The synthesis of nickel ferrite nanoparticles is accomplished through the sol-gel auto-combustion technique. Various analytical approaches are employed to confirm the formation of the developed material. A vector network analyzer is used to examine the materials' electromagnetic properties in order to evaluate their potential for use in defence applications. In addition to this, the developed composites are applied as a coating on a metal sheet and then further investigated. A vector network analyzer with free space approach is used to measure the reflection coefficient of the coated sheet in the frequency range of 2–18 GHz. Remarkably, the NC-2 composite exhibits a reflection coefficient exceeding −10 dB. The finding of this study highlight the potential of the nickel ferrite and activated charcoal composite as a promising candidate for microwave absorption in the X-Band.