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Nanocrystalline magnesium ferrite is synthesized at room temperature by high energy ball milling the MgO and α-Fe2O3 (1 : 1 mol fraction) powders. The Rietveld structure and microstructure refinements of X-ray powder diffraction data of 9 h milled sample reveal the presence of mixed and nearly inverse spinel nanocrystalline Mg-ferrite phases. Postannealing of nanocrystalline powder within 873–1473 K reveals continuous change in cation distribution among the tetrahedral and octahedral sites of mixed spinel lattice leading to nearly inverse spinel structure with increasing temperature. Mixed spinel structure finally transformed into inverse spinel structure after 1 h of annealing at 1073 K. The ferrite phase becomes completely stoichiometric by solid-state diffusion of unreacted (∼0.3 mol fraction) α-Fe2O3 into spinel lattice after 1 h of annealing at 1273 K. Interestingly, particle sizes of ferrite phases do not increase considerably up to 1073 K and increase suddenly after transformation of mixed spinel into nearly inverse spinel structure.

Microstructure Characterization of Nanocrystalline Magnesium Ferrite Annealed at Elevated Temperatures by Rietveld Method