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.

This study investigates the structural and magnetic properties of CoFe₂O₄ nanoparticles prepared by five different synthesis methods: coprecipitation, ultrasound-assisted coprecipitation, coprecipitation coupled with mechanochemical treatment, microemulsion and microwave-assisted hydrothermal synthesis. The produced powders were additionally functionalized with starch to improve biocompatibility and colloidal stability. The starch-coating procedure itself by sonication in starch solution, as well as its result, affects the structural and magnetic properties of functionalized nanoparticles. The resulting changes of properties in the process of ligand addition depend significantly on the starting nanoparticles, or rather, on the method of their synthesis. The structural, magnetic and spectroscopic properties of the resulting materials were systematically investigated using X-ray diffraction (XRD), Raman spectroscopy, Mössbauer spectroscopy and magnetic measurements. Taken together, XRD, Raman and Mössbauer spectroscopy show that starch deposition reduces structural disorder and internal stress, resulting in nanoparticles with a more uniform size distribution. These changes, in turn, affect all magnetic properties—magnetization, coercivity and magnetic anisotropy. Magnetic responses are preserved what is desirable for future biomedical applications. This work emphasizes the importance of surface modification for tailoring the properties of magnetic nanoparticles while maintaining their desired functionality.