57Fe Mössbauer spectra study of coated α-Fe2O3 nanoparticles

Nano-sized -Fe₂O₃ particles coated with polar organic molecules have been studied using the Mössbauer spectroscopy method. The -Fe₂O₃ nanoparticles were prepared by the microemulsion method. The average particle size of the Fe₂O₃ particles is about 24 Å. Because the particle size is so small that the Mössbauer spectra of the -Fe₂O₃ samples only consist of a quadrupole-split central line. It was proved that the Isomer Shifts (DIS) and the Quadrupole Splitting (DQS) changed as the refluxing time prolongs and the refluxing temperature increases during the preparation of the Fe₂O₃ nanoparticles, which implied an enhancement of the surface electrofield gradient formed by the surface coated polar molecules during the refluxing process.     

A Mössbauer study of the binary system LiNbO3-Fe2O3 in a broad concentration range

The binary system LiNbO₃-Fe₂O₃ has been studied by Mössbauer spectroscopy in the concentration range up to 24 mol% Fe₂O₃. For Fe₂O₃ concentrations up to 6 mol% iron is incorporated into the matrix of LiNbO₃ as Fe²⁺ and Fe³⁺, whereby the Fe²⁺ content decreases with increasing Fe₂O₃ concentration. Samples containing 9 and 11 mol% Fe₂O₃ showed only the Fe³⁺ valence state. There were no indications of any considerable formation of superparamagnetic Fe₂O₃ clusters up to 11 mol% Fe₂O₃. This is in agreement with the X-ray and DTA investigations of Takei and Katsumata (1982) who found that a solid solution exists between 0 and 11 mol% Fe₂O₃. Above 11 mol% the appearance of magnetically split sextets in the Mössbauer spectra indicated the formation of a second α-Fe₂O₃ phase. The isomer shift, which reflects the electron density at the Fe nucleus, measured as a function of the Fe₂O₃ concentration showed two steps, one at 6 mol% Fe₂O₃ (the turning point of the C_H axis parameter (Takei et al. 1982) and one at 11 mol% Fe₂O₃ (phase boundary). These steps were tentatively related to abrupt changes in the spontaneous polarization.     

Mössbauer study of magnetic order in RBa2Fe3O8

Complete replacement of copper by iron in RBa₂Cu₃O₇ leads to RBa₂Fe₃O₈ (R=Y, rare earth). Mössbauer spectroscopy measurements of⁵⁷Fe and¹⁵¹Eu in RBa₂Fe₃O₈ (R=Y, Eu, Ho, Er) at temperatures 4.2–800 K have been performed. Some of the spectra reveal two inequivalent iron sites, probably corresponding to iron in the Fe(2) site (fivefold oxygen coordination) and in the Fe(1) site (octahedral oxygen coordination). In all compounds the iron moments order antiferromagnetically at the same Néel temperatureT _N720 K. The¹⁵¹Eu Mössbauer spectra of EuBa₂Fe₃O₈ show that the Eu ion is trivalent and exposed to a small exchange field from the iron sublattices.     

Mössbauer investigation of non-aggregated γ-Fe2O3 particles

Investigation by Mössbauer spectroscopy of non-aggregated nanometric -Fe₂O₃ particles dispersed in polymer is reported. Magnetic interactions between the particles were controlled by varying the particle concentration in the polymer. The results show that over the investigated range, the interactions make the relaxation time shorter. Infield experiments show spin canting which increases with decreasing particle size.     

A Mössbauer effect study of MgFe2O4

A slowly cooled sample of the ferrimagnetic spinel MgFe₂O₄ has been studied with ⁵⁷Fe Mössbauer spectroscopy over a wide temperature range both with and without high magnetic fields. The observed temperature dependence of the A and B site hyperfine parameters is discussed. Conclusions about the spin structure, the magnetic exchange interactions and the supertransferred hyperfine fields are presented.     

Mössbauer study of carbon-supported α-Fe catalysts

Mössbauer spectra of carefully reduced carbon-supported iron catalysts show superparamagnetic -Fe at 80 K. The results indicate that the particle size depends on the reduction temperature. Effects of evacuation and CO chemisorption are discussed.     

A Mössbauer spectroscopic study of 3d magnetism of R2Fe14B

Guided by the occupancies and iron magnetic moments μ³, ⁵⁷Fe Mössbauer parameters of Y₂Fe₁₄B at 250K, and in turn for other temperatures, of the sublattices of iron were deduced. Plots of μ(T) in reduced coordinates, through the established correlation between hyperfine field Hn and μ, show that the corresponding state of different iron sites is different and all experimental points fall below Brillouin function. The relation between exchange integral deviation parameter Δ and standard deviation of Fe-Fe interatomic distances S is linear, indicating electrostatic nature of exchange interactions between spins in neighboring atoms. It is inclined to the view that fluctuations of exchange integral is responsible for low T_c of R₂Fe₁₄B.     

Mössbauer effect study of the Β-FeOOH to α-Fe2O3 phase transformation

-FeOOH was precipitated from a chloride solution. Mössbauer spectra were taken at room temperature (RT) and at 4.2 K in zero field and in external magnetic fields. Samples aged for successively longer time periods were studied. They contain -FeOOH and -Fe₂O₃, the Mössbauer spectra of which show superparamagnetic behavior. The transformation into -Fe₂O₃ is already induced by aging in the mother solution at 100 C. A final heat treatment at 350 C leads to the complete transformation into -Fe₂O₃ and to an increase of the crystallite size.     

Microwave absorption and Mössbauer studies of Fe3O4 nanoparticles

Materials consisting of nanometer-sized magnetic particles are currently the subject of intensive research activities. Especially, much attention has been paid to their promising features for microwave magnetic properties. Well dispersed Fe₃O₄ nanoparticles of 30 nm have been synthesized by oxidization method with NaNO₂, and the microwave magnetic properties of the composites have been studied. The real and imaginary part of relative permittivity remained low and nearly constant in the region of 0.1–18 GHz, respectively. As a result, the resin composites having a thickness of 2.0–3.2 mm, and containing 20 vol% Fe₃O₄ in the form of nanoparticles with an average diameter of 30 nm, exhibited excellent electromagnetic wave absorption properties in the frequency range of 4.5–12.0 GHz.     

Mössbauer spectroscopy of single-crystal LiNbO3:Fe(III)

Mössbauer spectra of LiNbO₃: Fe(III)-monocrystals in external magnetic fields of 0.3–7T with various configurations of the -direction, c-axis of the crystal, and the magnetic field direction are interpreted by means of a spin Hamiltonian. A consistent set of hyperfine and crystal-field parameters could be least squares fitted for all spectra. Arguments that Fe(III) substitutes Nb(V) are given.Work partly performed in ICEx/UFMG, Depto. de Fisica, Belo Horizonte, Brasil     

57Fe Mössbauer study of new multiferroic AgFeO2

The present work reports results of the ⁵⁷Fe Mössbauer measurements on AgFeO₂ powder sample recorded at various temperatures including the points of both magnetic phase transitions. The ⁵⁷Fe Mössbauer spectra of AgFeO₂ measured in the paramagnetic range (T > T _N1) consist of one quadrupole doublet with rather high quadrupole splitting of Δ_300K = 0.66 ± 0.01 mm/s for Fe³⁺ ions. In order to predict the sign of electric field gradient (EFG) at ⁵⁷Fe nuclei, we calculated the lattice contribution to the electric field gradient (EFG) at ⁵⁷Fe nuclei, which emphasized the importance of the dipolar contributions, with resultant oxygen polarizabilities in the range of α _O = 0.83 ų, in agreement with the results obtained previously for other delafossite-like oxides. In the temperature range of T _N2 < T < T _N1, Mössbauer spectra gave clear evidence for the existence of a distribution of the hyperfine magnetic fields H _hf at ⁵⁷Fe nuclei. We present the results of a model fitting of the spectra based on an assumption of the cycloid magnetic structure of AgFeO₂ at T < T _N2. The obtained data were analysed in comparison with published data on Mössbauer studies of oxide multiferroics.     

A Mössbauer study of rapidly quenchedCuFe alloys — Antiferromagnetic γ-Fe

A series ofCuFe alloys containing 5, 10 and 16 at% Fe has been prepared using standard ribbon spinning techniques. It is found that samples containing significant fractions ( 5%) of Fe in the form of r-Fe can be obtained readily on quenching from the (r + liquid) phase, applied field spectra (0–5.2 T) on antiferromagnetic r-Fe at 4. 2 K indicate that the anisotropy energy is small and that spins tilt from the minimum energy configuration (spin axes perpendicular to B_appl) for B_appl 2.5T.     

57Fe Mössbauer study of Lu2Fe3Si5 iron silicide superconductor

With the advent of Fe–As based superconductivity it has become important to study how superconductivity manifests itself in details of ⁵⁷Fe Mössbauer spectroscopy of conventional, Fe-bearing superconductors. To this end, the iron-based superconductor Lu₂Fe₃Si₅ has been studied by ⁵⁷Fe Mössbauer spectroscopy over the temperature range from 4.4 K to room temperature with particular attention to the region close to the superconducting transition temperature (T_c=6.1 K). Consistent with the two crystallographic sites for Fe in this structure, the observed spectra appear to have a pattern consisting of two doublets over the whole temperature range. The value of Debye temperature was estimated from temperature dependence of the isomer shift and the total spectral area and compared with the specific heat capacity data. Neither abnormal behavior of the hyperfine parameters at or near T_c, nor phonon softening were observed.     

Mössbauer study of Fe‐doped CuGeO3 system Cu0.9Ge0.9Fe0.2O3

The Fe‐doped system Cu_0.9Ge_0.9Fe_0.2O₃ has been investigated by means of X‐ray diffractometry, Mössbauer spectroscopy and superconducting quantum interference device. The structure of this system is orthorhombic and the lattice constants are a=4.784 Å, b=8.472 Å and c=2.904 Å, respectively. Magnetic measurements confirm that the spin‐Peierls transition appears in our sample at about 12 K, which is near to the spin‐Peierls transition temperature (T _sp) 14 K of pure CuGeO₃ system. The Mössbauer spectrum shows the superposition of two Zeeman sextets and a broad central line due to Fe³⁺ ions from room temperature to 4.2 K. The Mössbauer parameters show a discontinuity near T _sp. The jump of the magnetic hyperfine field at temperatures lower than T _sp means increasing of the superexchange interaction among the magnetic ions. The jump of the quadrupole splitting and the isomer shift values could be interpreted as due to decrement in symmetry of lattice sites and spontaneous thermal contraction.     

A magnetic and Mössbauer study of melt-spun Nd60Fe30Al10

Nd₆₀Fe₃₀Al₁₀ alloys were rapidly quenched by the melt-spinning technique with different wheel surface speeds ranging from 5 to 30 m/s. The microstructure and the magnetic properties were strongly dependent on the quenching rate. A high quenching rate led to an amorphous structure with a low coercivity at room temperature, while a mixture of amorphous and crystalline phases was found after melt-spinning at 5 m/s, which exhibited hard magnetic properties at room temperature. For both the ribbons melt-spun at 5 and 30 m/s respectively, coercivity increased with decreasing temperature and reached a maximum at around 50 K. Maximum magnetization at 10 T increased dramatically at low temperature. Our magnetic study has shown that the presence of crystalline Nd was responsible for the increase of magnetization and the decrease of coercivity, as Nd became magnetically ordered at low temperatures. The Mössbauer study has shown that the magnetic microstructures of melt-spun ribbons were not uniform, as the spectra needed to be fitted by magnetic and non-magnetic components.     

Mössbauer spectroscopy study on the hydrothermal transformation α-FeOOH→α-Fe2O3

The reaction kinetics of the hydrothermal transformation -FeOOH-Fe₂O₃ was studied by means of Mössbauer spectroscopy. From the reaction isotherms, a monomolecular, first order reaction was found to characterise the hydrothermal transformation of alpha oxihydroxide to the alpha iron oxide. The rate constant as well as the activation energy of this process were determined. No intermediate phases were identified in the hydrothermal samples. The thermodynamic properties of the hydrothermal system -FeOOH-Fe₂O₃ in correlation with Mössbauer spectroscopy data are discussed.     

In situ high-pressure study of LiNbO3-type FeTiO3: X-ray diffraction and Mössbauer spectroscopy

The structure of LiNbO₃-type FeTiO₃ and the oxidation state of Fe have been investigated using X-ray diffraction and Mössbauer spectroscopy in the diamond anvil cell up to 18 GPa at room temperature. A structural phase transition is observed at 15.7 GPa from LiNbO₃-type to perovskite-type, accompanied by a volume collapse of 1.5%. LiNbO₃-type FeTiO₃, which is shown to contain only ferrous iron up to this pressure, and no charge transfer is observed. In addition to the c/a axial ratio that has been used to distinguish between ilmenite and LiNbO₃-type FeTiO₃, the hyperfine parameters (isomer shift and quadrupole splitting) provide an efficient way to discriminate between these two phases.     

Mössbauer study of a Fe3O4/PMMA nanocomposite synthesized by sonochemistry

Magnetite nanoparticles of 10 nm average size were synthesized by ultrasonic waves from the chemical reaction and precipitation of ferrous and ferric iron chloride (FeCl₃ · 6H₂O y FeCl₂ · 4H₂O) in a basic medium. The formation and the incorporation of the magnetite in PMMA were followed by XRD and Mössbauer Spectroscopy. These magnetite nanoparticles were subsequently incorporated into the polymer by ultrasonic waves in order to obtain the final sample of 5 % weight Fe₃O₄ into the polymethylmethacrylate (PMMA). Both samples Fe₃O₄ nanoparticles and 5 % Fe₃O₄/PMMA nanocomposite, were studied by Mössbauer spectroscopy in the temperature range of 300 K–77 K. In the case of room temperature, the Mössbauer spectrum of the Fe₃O₄ nanoparticles sample was fitted with two magnetic histograms, one corresponding to the tetrahedral sites (Fe^3?+?) and the other to the octahedral sites (Fe^3?+? and Fe^2?+?), while the 5 % Fe₃O₄/PMMA sample was fitted with two histograms as before and a singlet subspectrum related to a superparamagnetic behavior, caused by the dispersion of the nanoparticles into the polymer. The 77 K Mössabuer spectra for both samples were fitted with five magnetic subspectra similar to the bulk magnetite and for the 5 % Fe₃O₄/PMMA sample it was needed to add also a superparamagnetic singlet. Additionally, a study of the Verwey transition has been done and it was observed a different behavior compared with that of bulk magnetite.