Size-controlled synthesis of spinel nickel ferrite nanorods by thermal decomposition of a bimetallic Fe/Ni-MOF

In this work, size-controlled synthesis of nickel ferrite nanoparticles was achieved by the calcination of a bimetallic (Fe/Ni) metal-organic framework (MOF). The bimetallic MOF (Fe₂Ni-MIL-88B) itself was prepared by a two-step route. The first step involved synthesis of the secondary building unit (SBU) by reacting stoichiometric amounts of Ni and Fe precursors with acetic acid. A ligand substitution reaction (terephthalate replaces acetate) in the SBU leads to the formation of the MOF, which was characterized by PXRD, FTIR, SEM and TEM. Afterwards, the MOF was calcined under air atmosphere to obtain nickel ferrite nanorods. PXRD analysis confirmed the spinel structure of the nickel ferrites while electron microscopic analysis (SEM, TEM) revealed their nanorod-like morphology. By increasing the calcination temperature from 600 to 1000 °C, particle size increased from 16 to 32 nm. Oxidation of benzyl alcohol was used as a model test reaction to probe the applicability of spinel nickel ferrite nanorods for catalysis. Interestingly, the largest nanorods exhibited the highest activity (86% conversion), thus demonstrating the potential of spinel ferrites in catalyzing oxidation reactions.