The present work reports the impact of sintering conditions on the phase stability in hydroxyapatite (HA)−magnetite (Fe 3 O 4 ) bulk composites, which were densified using either pressureless sintering in air or by rapid densification via hot pressing in inert atmosphere. In particular, the phase abundances, structural and magnetic properties of the (1−x)HA-xFe 3 O 4 (x = 5, 10, 20, and 40 wt %) composites were quantified by corroborating results obtained from Rietveld refinement of the X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Mossbauer spectroscopy. Post heat treatment phase analysis revealed a major retention of Fe 3 O 4 in argon atmosphere, while it was partially/completely oxidized to hematite (α-Fe 2 O 3 ) in air. Mossbauer results suggest the hightemperature diffusion of Fe 3+ into hydroxyapatite lattice, leading to the formation of Fe-doped HA. A preferential occupancy of Fe 3+ at the Ca(1) and Ca(2) sites under hot-pressing and conventional sintering conditions, respectively, was observed. The lattice expansion in HA from Rietveld analysis correlated well with the amounts of Fe-doped HA determined from the Mossbauer spectra. Furthermore, hydroxyapatite in the monoliths and composites was delineated to exist in the monoclinic (P2 1 /b) structure as against the widely reported hexagonal (P6 3 /m) crystal lattice. The compositional similarity of iron doping in hydroxyapatite to that of tooth enamel and bone presents HA-Fe 3 O 4 composites as potential orthopedic and dental implant materials.
We report the origin of room temperature weak ferromagnetic behavior of polycrystalline Pb(Fe 2/3 W 1/3 )O 3 (PFW) powder. The structure and magnetic properties of the ceramic powder prepared by a Columbite method were characterized by X-ray and neutron diffraction, Mössbauer spectroscopy and magnetization measurements. Rietveld analysis of diffraction data confirm the formation of single phase PFW, without traces of any parasitic pyrochlore phase. PFW was found to crystallize in the cubic structure at room temperature. The Rietveld refinement of neutron diffraction data measured at room temperature confirmed the G-type antiferromagnetic structure of PFW in our sample. However, along with the antiferromagnetic (AFM) ordering of the Fe spins, we have observed the existence of weak ferromagnetism at room temperature through: (i) a clear opening of hysteresis (M-H) loop, (ii) bifurcation of the field cooled and zero-field cooled susceptibility; supported by Mössbauer spectroscopy results. The P-E loop measurements showed a non-linear slim hysteresis loop at room temperature due to the electronic conduction through the local inhomogeneities in the PFW crystallites and the inter-particle regions. By corroborating all the magnetic measurements, especially the spin glass nature of the sample, with the conduction behavior of the sample, we report here that the observed ferromagnetism originates at these local inhomogeneous regions in the sample, where the Fe-spins are not perfectly aligned antiferromagnetically due to the compositional disordering.
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