The series of nanoparticles of iron-cobalt spinel (FexCo3−xO4) covering a wide range of nominal compositions (x = 0.5; 1; 1.5; 2; 2.5), was prepared by applying a modified procedure described by Wu et al. [23]. The mixed spinel active phase was in situ deposited on doped mesoporous carbon support (N,S-MPC) using the microwave-assisted hydrothermal route. The corresponding transition metal precursor salts, Co(NO3)2·6H2O and Fe(NO3)3·9H2O, were dissolved in 3.5 cm3 distilled water in the appropriate molar ratio and stirred for 30 min. After heating the solution to 80 °C, 1.5 cm3 of 25 wt.% ammonia was added and stirred for the 30 min at this temperature. The prepared mixture was next added to a carbon suspension (0.01 g C/1 cm3 EtOH), and ultrasonicated for 15 min. The resultant mixture was then transferred to a Teflon lined microwave autoclave (Ertec/MAGNUM II, Wrocław, Poland). The reaction temperature was kept at 150 °C for 30 min. The products were centrifuged and washed several times with distilled water and ethanol, and then dried at a temperature of 80 °C overnight. The obtained final catalysts (iron-cobalt spinel deposited on the N,S-MPC support) is labeled as Fe-Co_x/N,S-MPC, where x determines the iron content in the sample, e.g., for x = 0.5 − Fe-Co_0.5/N,S-MPC. For the sake of comparison cobalt spinel (Co3O4) deposited on doped mesoporous carbon support was synthesized (denoted Co/N,S-MPC) according to the same procedure described elsewhere. The Co/N,S-MPC catalyst was used as reference material.
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