In this paper, Ternary composites of polyaniline/NiZn ferrite/carbonyl iron (PANI/F/CI) are prepared via two stages: Firstly, Ni0.5Zn0.5Fe2O4 is prepared using a sol-gel method while carbonyl iron is commercially purchased. After that, PANI/F/CI composites are prepared using an in-situ polymerization technique of PANI in the existence of the Ni0.5Zn0.5Fe2O4 and CI. X-ray diffractometry, FTIR spectroscopy, UV-vis spectroscopy, TGA analysis, and SEM analysis are utilized in order to characterize samples. The morphology of the powders is investigated by SEM. The electromagnetic interference shielding and microwave absorption properties are measured in the frequency band of 8.8–12 GHz to investigate the microwave characterization. The results refer those microwave absorption properties are related to the absorber thickness and the loading ratio of the absorber within a paraffin matrix. Minimal reflection loss of -30.8 dB at the matching frequency of 10.3 GHz and the absorption bandwidth under − 10 dB of 2.8 GHz for 3.4 mm thickness with a surface density of 3.38 kg/m2 are noticed for the PANI/F/CI composite sample. The maximum shielding efficiency of 30.12 dB at 11.0 GHz for 3.2 mm thickness is observed for the PANI/F/CI composite sample.