| Summary: | Co<sub>1−<i>x</i></sub>Zn<i><sub>x</sub></i>Fe<sub>2</sub>O<sub>4</sub> nanoparticles (0 ≤ <i>x</i> ≤ 1) have been synthesized via a green sol–gel combustion method. The prepared samples were studied using X-ray diffraction measurements (XRD), transmission electron microscopy (TEM), Raman, and magnetic measurements. All samples were found to be single phases and have a cubic <i>Fd-3m</i> structure. EDS analysis confirmed the presence of cobalt, zinc, iron, and oxygen in all studied samples. Raman spectra clearly show that Zn ions are preferentially located in T sites for low Zn concentrations. Due to their high crystallinity, the nanoparticles show high values of the magnetization, which increases with the Zn content for <i>x</i> < 0.5. The magnetic properties are discussed based on Raman results. Co ferrite doped with 30% of Zn produced the largest SAR values, which increase linearly from 148 to 840 W/g<sub>MNPs</sub> as the H is increased from 20 to 60 kA/m.
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