Synthesis and characterization of Co–Fe nanoparticles supported on mesoporous silicas

Co–Fe bimetallic samples containing 25 wt% total of metal content were prepared by incipient wetness impregnation of cobalt nitrate and iron nitrate salts over hexagonal mesoporous silica (HMS) and SBA-15 supports. Changes in the textural properties and reduction behavior were compared with monometallic cobalt/iron-based samples. The samples were characterized by N2 physisorption, X-ray diffraction (XRD), H2-temperature programmed reduction (TPR), transmission electron microscopy (TEM) and H2 chemisorption. The amount of incorporated metal was estimated by atomic absorption spectroscopy (AAS). Morphological properties revealed that after introduction of the metal to the SBA-15 support, the specific area, pore volume and pore diameter decreased to a lesser extent for bimetallic samples. XRD measurements detected the formation of Co3O4 and CoFe2O4 phases for both bimetallic samples. TPR profiles indicated similar behavior for both the bimetallic and monometallic samples. Higher temperatures were observed for the reducibility of Co–Fe/HMS as compared to Co–Fe/SBA-15. Dispersion values of the bimetallic samples were higher than Fe monometallic samples and lower than Co monometallic samples according to hydrogen chemisorption. The particle size distribution of the bimetallic samples estimated by TEM microphotographs showed a smaller fraction of larger size particles for Co–Fe/SBA-15. - Highlights: ► Co–Fe samples supported on both SBA-15 and HMS mesoporous silicas were obtained. ► Co–Fe/HMS and Co–Fe/SBA-15 samples presented Co3O4 (cubic) and CoFe2O4 (cubic) phases. ► Co is lesser reduced than Fe in bimetallic samples. ► Co–Fe/HMS and Co–Fe/SBA-15 presented great mechanical stability. ► Bimetallic samples revealed smaller particles than the monometallic ones