The present study managed to build, nanocomposites (NCs) containing nickel ferrite and functionalized multi-walled carbon nanotubes (NiFe2O4@MWCNTs) with different weight to ratios absorb electromagnetic waves (EM) in the X and Ku bands. In addition, the structural and electromagnetic (EM) properties of the nanocomposites were characterized. In the first step, NiFe2O4 nanoparticles (NFNPs) were successfully synthesized via a citrate-nitrate (C–N) method. Subsequently, NFNPs and MWCNTs were blended at various weight ratios to form NF@MWCNTs nanocomposites. The X-ray diffraction (XRD) was used to determine the crystal structure. Field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS) were used for surface morphology and elemental analysis. Transmission electron microscopy (TEM) was used to describe the distribution of NFNPs on the MWCNTs surface. Infrared (IR) and vibrating sample magnetometer (VSM) were used to examine the magnetic properties. The vector network analyzer (VNA) was used to examine the absorption properties of EM waves. The properties of NF@MWCNTs nanocomposites were examine at five different weight ratios. The S3 sample with a thickness of 2.00 mm exhibited the best loss in the X band, reaching −30.47 dB. Furthermore, the S2 sample with a thickness of 5.00 mm exhibited the lowest Ku-band loss, reaching a value of −17.39 dB.