Herein, we report on developing a facile synthetic route for reusable nanocatalysts based on a combination of the supermagnetic properties of magnetite with the unique optical and catalytic properties of noble metal hybrid nanomaterials. We compare two different synthetic methods, to find out which is best from synthetic and application points of view, for the synthesis of Fe₃O₄ and Fe₃O₄@M (M = Ag or Au) core-shell hybrid nanostructures. The two different single-step synthetic methods are: thermal decomposition and hydrothermal. The structural, morphological and magnetic properties of the obtained Fe₃O₄ and Fe₃O₄@M nanoparticles were characterized by various techniques. XRD of the Fe₃O₄ nanoparticles exhibited sharp and strong diffraction peaks, confirming the highly crystalline structure of the Fe₃O₄ particles synthesized by the hydrothermal method, while broad and weak peaks were observed on using the thermal decomposition method. Both Fe₃O₄@Ag and Fe₃O₄@Au core-shells obtained by the hydrothermal method showed the reflection planes of Fe₃O₄ and additional planes of Ag or Au. But on the formation of Fe₃O₄@Ag/Au by the thermal decomposition method the peak for Fe₃O₄ disappeared and only the diffraction peaks of Ag or Au appeared. According to TEM analysis there was a broad particle-size distribution, random near-spherical shapes and slight particle agglomeration for Fe₃O₄ synthesized by the thermal decomposition method. However, there was a moderate size distribution, spherical shapes and well-dispersed particles without large aggregations for the hydrothermal method. TEM images of the synthesized nanoparticles by the two methods used showed a pronounced difference in both size and morphological shape. The catalytic performance of the synthesized nanoparticles was examined for the reduction of Congo red dye in the presence of NaBH₄. The Fe₃O₄ nanocatalyst maintained its catalytic activity for only one cycle. In the cases of Fe₃O₄@Au and Fe₃O₄@Ag, the catalytic activity was conserved for four and ten successive cycles, respectively. Based on the obtained results, it was concluded that the hydrothermal synthesis of Fe₃O₄, Fe₃O₄@Ag and Fe₃O₄@Au nanostructures is highly recommended due to their selectivity and merits.

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