A Structural and Magnetic Investigation of the Inversion Degree in Spinel NiFe2O4, ZnFe2O4 and Ni0.5Zn0.5Fe2O4 Ferrites Prepared by Soft Mechanochemical Synthesis

NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Chitosan Functionalized Fe3O4@Au Core-Shell Nanomaterials for Targeted Drug Delivery

Chitosan functionalized Fe3O4-Au core shell nanoparticles have been prepared using a two-step wet chemical approach using NaBH4 as reducing agent for formation of Au in ethylene glycol. X-ray diffraction studies shows individual phases of Fe3O4 and Au in the as prepared samples with crystallite size of 5.9 and 11.4 nm respectively. The functionalization of the core-shell nanostructure with Chitosan has been confirmed using Fourier transform infrared spectroscopy along with signatures of octahedral and tetrahedral sites of Fe3O4 below 600cm-1. Mössbauer spectroscopy shows decrease in particle-particle interaction in presence of Au shell (72% sextet) than pure oleic coated Fe3O4 nanoparticles (88% sextet) at room temperature. At 80K, oleic acid coated Fe3O4 shows only sextets whereas the Chitosan functionalized Fe3O4 and Chitosan functionalized Fe3O4@Au core shell show presence of 5 and 11% doublet, respectively.

Structure and Magnetic Properties of Nanocomposite Fe2O3/TiO2 Catalysts Fabricated by Heterogeneous Precipitation

The aim of our work is to study phase composition, particle size and magnetic response of Fe2O3/TiO2 nanocomposites with respect to the final annealing temperature. Those nanomaterials are considered as smart catalysts, separable from a liquid/gaseous phase by applied magnetic field. The starting product was obtained by an ecologically acceptable route, based on heterogeneous precipitation of the TiO2 on modified g-Fe2O3 nanocrystals dispersed in water. The precursor was subsequently annealed on air at temperatures ranging from 200 oC to 900 oC. The samples were investigated by synchrotron X-ray powder diffraction (S-PXRD), magnetic measurements and Mössbauer spectroscopy. As evidenced by S-PXRD and Mössbauer spectroscopy, increasing the annealing temperature causes evolution of the phase composition from anatase/maghemite to rutile/hematite, finally above 700 oC the pseudobrookite (Fe2TiO5) also forms. The apparent particle size of the various Fe2O3/TiO2 phases has been determined from the highquality S-PXRD data by using two different approaches: the Rietveld refinement and the Debye method. Magnetic response of the samples is discussed in considering the phase composition and the particle size.