This research examines the structural and magnetic properties of monodomain cobalt ferrite nanoparticles with the formula (Co_1−xFe_x)^A[Fe_2−xCo_x]^BO₄. The particles were synthesized using various methods, including coprecipitation (with and without ultrasonic assistance), coprecipitation followed by mechanochemical treatment, microemulsion, and microwave-assisted hydrothermal techniques. The resulting materials were extensively analyzed using X-ray diffraction (XRD) and magnetic measurements to investigate how different synthesis methods affect the structure and cation distribution in nanoscale CoFe₂O₄. For particles ranging from 15.8 to 19.0 nm in size, the coercivity showed a near-linear increase from 302 Oe to 1195 Oe as particle size increased. Saturation magnetization values fell between 62.6 emu g⁻¹ and 74.3 emu g⁻¹, primarily influenced by the inversion coefficient x (0.58–0.85). XRD analysis revealed that as the larger Co²⁺ cations migrate from B- to A-sites (decreasing x), the lattice constants and inter-cation hopping distances increase, while the average strength of super-exchange interactions decreases. This study establishes a connection between the magnetic properties of the synthesized samples and their structural features. Importantly, this research demonstrates that careful selection of the synthesis method can be used to control the magnetic properties of these nanoparticles.