<p>Nickel cobalt ferrites, a single and pure phase material with nanoscale particle dimensions, were fabricated through the thermal breakdown of a precursor compound with the molecular formula Ni_xCo_1−xFe₂(C₄H₄O₄)₃·6N₂H₄, where x had values of 0.2, 0.4, 0.6, and 0.8. The CHNS analysis and metal analysis established the composition and formula of the precursor. The technique of infrared spectroscopy verified that the metals are bound to the succinate through a single-point linkage, whereas the hydrazine ligands form a bridge bond between the two metals. The breakdown patterns of the precursors were elucidated using data from various thermal analysis methods. The precursor exhibits pyrophoric characteristics and, upon ignition, undergoes a slow, controlled combustion reaction to produce pure, nanoscale ferrites. Powder X-ray diffraction analysis confirmed the formation of the cubic spinel phase, and Infrared and Raman spectroscopy verified the presence of M–O bonds at both MO₄-tetrahedra and MO₆ octahedra within the ferrites lattice. X-ray photoelectron spectroscopy (XPS) analysis revealed that nickel and cobalt are in the +2 oxidation state, whereas iron is in the +3 oxidation state. Electron microscopy images showed that the ferrites had a cuboidal shape. As the nickel concentration was altered, we noticed a reduction in the unit cell dimensions. A rise in Ni concentration led to a corresponding change in the magnetic properties of the ferrite, with its hardness notably decreasing as the concentration of Ni increased, whereas the Curie temperature exhibited an increase with the addition of Ni. The results of the dielectric constant study uncovered the significant potential of these materials for use in electronic devices. </p>