Iron oxide nanoparticles in NaA zeolite cages

Abstract

Zeolite NaA samples with varying concentration of Fe3+ ions have been prepared by wet chemical method. Based on powder X-ray diffraction, 29Si and 27Al MAS NMR and Fe3+ EPR investigations, the formation of nano-sized ferric oxide particles inside the larger α-cages of zeolite NaA has been established. Both Mössbauer effect and magnetization measurements carried out down to 4.5 K established the superparamagnetic behaviour of these Fe2O3 particles with a blocking temperature of ≈20 K, where the magnetization values showed deviation for the zero field cooled and field cooled samples and the appearance of a very narrow magnetic hysteresis loop below this temperature. For all Fe3+ containing samples the room temperature Mössbauer spectrum is a broad quadrupole doublet with chemical shift, δ ≈ 0.33 mm/s and quadrupole splitting, ΔEq ≈ 0.68 mm/s. Variable temperature 57Fe Mössbauer effect measurements exhibited magnetic features below the blocking temperature and at 4.5 K, the observed spectrum is a broad magnetic sextet characterized by an internal hyperfine field value of ≈504 kOe along with a very weak central superparamagnetic quadrupole doublet.