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The Co substitution in Ni-Zn ferrites with respect to their structural and magnetic properties has been investigated in favor to select a material for future electromagnetic interference (EMI) shielding application purpose. Ni 0.6−x Zn 0.4 Co x Fe 2 O 4 (x = 0, 0.03, 0.09, 0.27) nanoparticles were synthesized using a sol-gel method and annealed at 700 • C. The prepared Ni 0.6−x Zn 0.4 Co x Fe 2 O 4 samples were characterized for their structural, stoichiometric, and magnetic properties. X-ray diffraction patterns reveal the formation of single-phase spinel cubic structure formed at x = 0.27. The influence of Co doping on structural properties of Ni-Zn ferrite was examined with X-ray diffraction and field emission scanning electron microscopy. The stoichiometry of prepared samples has also been examined by energy-dispersive X-ray spectroscopy. The magnetic behavior was studied using a vibrating sample magnetometer at room temperature. The variations in values of saturation magnetization were explained on the basis of spin canting effect imparted by hematite (α-Fe 2 O 3 ) phase with spinel phase. Ni 0.6−x Zn 0.4 Co x Fe 2 O 4 with x = 0.27 possesses best saturation magnetization and can be useful in EMI shielding material.