Hard‐magnetic CoFe2O4 nanoparticles were produced with the sol‐gel autocombustion route using agarose and citric acid as a neutral organic gel and combustion agent. For this purpose, the obtained gel is annealed at 800°C for 3 hours and then the spinel structure of the samples was confirmed by X‐ray diffraction (XRD). In addition, the existence of metal‐oxygen complexes in the gel and nanoparticles was investigated by Fourier transformation infrared (FTIR) spectra. Furthermore, FESEM images showed that semispherical and rod‐like particles were obtained by variation in agarose contents. For the rod‐like sample with 2.5 g agarose, the saturation magnetization and coercivity were measured equal to 71.7 emu/g and 10076.84 Oe, respectively.