Controlled reduction of LaFe xMn yMo zO3/Al2O3 composites to produce highly dispersed and stable Fe0 catalysts: a Mössbauer investigation

In this work, controlled reduction of perovskites supported on Al2O3 was used to prepare thermally stable nanodispersed iron catalysts based on Fe0/La2O3/Al2O3. The perovskites composites LaFe0.90Mn0.08Mo0.02O3(25, 33 and 50 wt (%)) /Al2O3 and LaFe0.90Mn0.1O3(25 wt (%)) /Al2O3 were prepared and characterized by XRD, BET, TPR, SEM and Mössbauer spectroscopy. XRD for unsupported perovskite showed the formation of a single phase perovskite structure. The Mössbauer spectra of the perovskites were fitted with hyperfine field distribution model for the perovskite. Supported perovskites on Al2O3 showed a decrease of the hyperfine field in respect to unsupported perovskite, due to decrease of particle size and dispersion of the Fe3+ specimens on the support. Also showed broaden lines and relaxation effects due to the small particle size. To produce the Fe0 catalyst, the composite perovskite(25%)/Al2O3 was reduced with H2 at 900, 1000 and 1100 °C for 1 hour. XRD data indicated the formation of Fe0 catalyst with particles sizes of ca. 35 nm. The Mössbauer spectrum showed the formation of metallic iron and doublets corresponding to species of octahedric Fe2+ and Fe3+ sites dispersed on Al2O3. These catalysts showed improved stability towards sintering even upon treatment at 1000 and 1100 °C under H2.