Abstract: 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.
Abstract: 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.
Abstract: 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.