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In this paper, the techniques for the synthesis of CaFe₂O₄ nanoparticles using the auto-combustion and co-precipitation methods are discussed. The effects of both methods on the microstructure and magnetic properties of the CaFe₂O₄ nanoparticles were compared. The CaFe₂O₄ powder was obtained after drying the synthesized sample via co-precipitation overnight in an oven at 80 °C. For auto-combustion method, the sol that was initially formed was gradually converted into a gel, which was then combusted at 250 °C. Finally, the CaFe₂O₄ nanoparticles were calcined at 550 °C. The different synthesis methods produced nanoparticles with different physical and magnetic properties in order to find an optimum size to be utilized for drug delivery applications. The results of the X-ray diffraction showed that both processes produced nanocrystals with an orthorhombic crystalline structure. It was noted from the …