Concerning the cation distribution in MnFe2O4 synthesized through the thermal decomposition of oxalates

A single phase manganese ferrite powder have been synthesized through the thermal decomposition reaction of MnC₂O₄·2H₂O-FeC₂O₄·2H₂O (1:2 mole ratio) mixture in air. DTA-TG, XRD, Mössbauer spectroscopy, FT-IR and SEM techniques were used to investigate the effect of calcination temperature on the mixture. Firing of the mixture in the range 300-500 °C produce ultra-fine particles of α-Fe₂O₃ having paramagnetic properties. XRD, Mössbauer spectroscopy as well as SEM experiments showed the progressive increase in the particle size of α-Fe₂O₃ up to 500 °C. DTA study reveals an exothermic phase transition at 550 °C attributed to the formation of a Fe₂O₃-Mn₂O₃ solid solution which persists to appear up to 1000 °C. At 1100 °C, the single phase MnFe₂O₄ with a cubic structure predominated. The Mössbauer effect spectrum of the produced ferrite exhibits normal Zeeman split sextets due to Fe³⁺ions at tetrahedral (A) and octahedral (B) sites. The obtained cation distribution from Mössbauer spectroscopy is (Fe_0.92Mn_0.08)[Fe_1.08Mn_0.92]O₄.     

Mössbauer study of Na0.82Co0.99Fe0.01O2

We studied by Mössbauer spectroscopy the Na_0.82CoO₂ compound using 1% ⁵⁷Fe as a local probe which substitutes for the Co ions. Mössbauer spectra at T=300 K revealed two sites which correspond to Fe³⁺ and Fe⁴⁺. The existence of two distinct values of the quadrupole splitting instead of a continuous distribution should be related with the charge ordering of Co⁺³, Co⁺⁴ ions and ion ordering of Na(1) and Na(2). Below T=10 K part of the spectrum area, corresponding to Fe⁴⁺ and all of Fe³⁺, displays broad magnetically split spectra arising either from short-range magnetic correlations or from slow electronic spin relaxation.     

Mössbauer study of antiferromagnetic CuFeO2

We have studied the magnetic spin structure of antiferromagnetic CuFeO₂ by X-ray diffraction (XRD) and Mössbauer spectroscopy. Its crystal structure determined by XRD analysis was a rhombohedral structure (space group R-3m) and lattice constants a₀ and c₀ were 3.0333 and 17.1595 Å, respectively. In spite of 4-Fe sublattices in a delafossite CuFeO₂, its Mössbauer spectra were analyzed with 1-set (6-Lorentzian lines) below 10 K due to the collinear-commensurate spin structure, but the spectra were fitted with 4-sextet above 10 K due to the incommensurate spin structure. This phenomenon was attributed to the spin–lattice relaxation effect. Magnetic Néel temperature was also determined at 18 K, which corresponded to the high-spin Fe³⁺ valance state. On the other hand, CuFe_0.98Al_0.02O₂ powder with a noncollinear spin structure was fitted with 4-sextet at 4.2 K.     

Effects of annealing temperature on structure and magnetic properties of CoAl0.2Fe1.8O4/SiO2 nanocomposites

CoAl_0.2Fe_1.8O₄/SiO₂ nanocomposites were prepared by sol–gel method. The effects of annealing temperature on the structure and magnetic properties of the samples were studied by X-ray diffraction, transmission electron microscopy, vibrating sample magnetometer and Mössbauer spectroscopy. The results show that the CoAl_0.2Fe_1.8O₄ in the samples exhibits a spinel structure after being annealed. As annealing temperature increases from 800 to 1200 °C, the average grain size of CoAl_0.2Fe_1.8O₄ in the nanocomposites increases from 5 to 41 nm while the lattice constant decreases from 0.8397 to 0.8391 nm, the saturation magnetization increases from 21.96 to 41.53 emu/g. Coercivity reaches a maximum of 1082 Oe for the sample annealed at 1100 °C, and thereafter decreases with further increasing annealing temperature. Mössbauer spectra show that the isomer shift decreases, hyperfine field increases and the samples transfer from mixed state of superparamagnetic and magnetic order to the completely magnetic order with annealing temperature increasing from 800 to 1200 °C.     

Investigating the formation and magnetic properties of the Dy0.75Fe1.25O3 orthoferrite prepared by sol-gel method

In this paper, the Dy_0.75Fe_1.25O₃ orthoferrite nanoparticles were synthesized successfully by sol-gel method. Dy_0.75Fe_1.25O₃ orthoferrite nanoparticles are obtained by calcining the flakes at 600 and 700 °C. The magnetic properties of the different samples are investigated using Quantum Design MPMS SQUID magnetometer and MS-500 Mössbauer spectrometer. Magnetic phase γ-Fe₂O₃ coexists in the samples calcined at 600 °C and orthoferrite phase is completely recovered in the samples calcined at 700 °C. Although excessive Fe³⁺ ions were introduced, none of these iron spins couple magnetically with Dy³⁺ ions.     

Recoilless fraction, structural, magnetic and thermal properties of Fe73.5Cu1Nb3Si13.5B9 alloy

Differential scanning calorimetry, X-ray diffraction and room temperature Mössbauer spectrum measurements of Fe_73.5Cu₁Nb₃Si_13.5B₉ (Finemet) alloy have been carried out in order to study its structural and magnetic properties as a function of annealing temperature. The DSC profile of as-quenched Finemet showed two exothermic peaks at 530 and 702 °C, corresponding to two crystallization processes. The Finemet alloy remains amorphous at 450 °C with one broad peak in XRD pattern and one broad sextet in Mössbauer spectrum. When the Finemet alloy was annealed at 550 °C, only well indexed body-center-cubic phase was detected. After being annealed at 650 and 750 °C, the XRD patterns showed the coexistence of α-Fe(Si) and Fe-B intermetallic phases with the increase in XRD peak intensities, indicating the growth of crystallites and the decomposition of Fe_73.5Cu₁Nb₃Si_13.5B₉ alloy at elevated temperatures. The Mössbauer spectra of annealed Finemet alloy could be fitted with 4 or 5 sextets and one doublet at higher annealing temperatures, revealing the appearance of different crystalline phases corresponding to the different Fe sites above the crystallization temperature. The appearance of the nanocrystalline phases at different annealing temperatures was further confirmed by the recoilless fraction measurements.     

Magnetic properties of Co-ferrite-doped hydroxyapatite nanoparticles having a core/shell structure

The magnetic properties of Co-ferrite-doped hydroxyapatite (HAP) nanoparticles of composition Ca_10−3xFe_2xCo_x(PO₄)₆(OH)₂ (where x=0, 0.1, 0.2, 0.3, 0.4 and 0.5% mole) are studied. Transmission electron microscope micrograms show that the 90 nm size nanoparticles annealed at 1250 °C have a core/shell structure. Their electron diffraction patterns show that the shell is composed of the hydroxyapatite and the core is composed of the Co-ferrite, CoFe₂O₄. Electron spin resonance measurements indicate that the Co²⁺ ions are being substituted into the Ca(1) sites in HAP lattice. X-ray diffraction studies show the formation of impurity phases as higher amounts of the Fe³⁺/Co²⁺ ions which are substituted into the HAP host matrix. The presence of two sextets (one for the A-site Fe³⁺ and the other for the B-site Fe³⁺) in the Mössbauer spectrum for all the doped samples clearly indicates that the CoFe₂O₄.cores are in the ferromagnetic state. Evidence of the impurity phases is seen in the appearance of doublet patterns in the Mössbauer spectrums for the heavier-doped (x=0.4 and 0.5) specimens. The decrease in the saturation magnetizations and other magnetic properties of the nanoparticles at the higher doping levels is consistent with some of the Fe³⁺ and Co²⁺ which being used to form the CoO and Fe₂O₃ impurity phase seen in the XRD patterns.     

Influence of aluminum doping in Li–Co–Ti ferrite

The crystallographic and magnetic properties of low aluminum doped lithium cobalt titanium ferrites, Li_0.5Co_0.2Ti_0.2Al_xFe_2.1−xO₄(0.0≤x≤0.5), in the scope of spinel structure and ferrimagnetic property were investigated. Ferrites were doped with aluminum in the range of 0.0–0.5 and were synthesized by using the conventional ceramic methods. Using X-ray diffraction and Mössbauer spectroscopy, we confirmed the formation of crystallized particles. All of the samples showed a single phase with a spinel structure, and the lattice parameters linearly decreased as the doped aluminum content was increased. The particle size of the samples also decreased as the doped aluminum content increased. Until x=0.4 in Li_0.5Co_0.2Ti_0.2Al_xFe_2.1−xO₄, the Mössbauer spectra could be fitted with two Zeeman sextets, which is the typical spinel ferrite spectra of Fe³⁺ with A- and B-sites. However, for x=0.5, the Mössbauer spectrum could be fitted with two Zeeman sextets and one doublet. From the variation of the Mössbauer parameters and the absorption area ratio, the cation distributions were determined. The magnetic behavior of the samples showed that an increase in the aluminum contents led to a decrease in the saturation magnetization, whereas the coercivity decreased until x=0.4 and then increased. The minimum coercivity was 52.4 Oe at x=0.4 in Li_0.5Co_0.2Ti_0.2Al_xFe_2.1−xO₄.     

Critical behaviour and magnetic properties of A-B spinel ZnxCu1−xFe2O4

Polycrystalline Zn_0.6Cu_0.4Fe₂O₄ ferrites have been prepared using a solid-state reaction technique. Their structural and magnetic properties have been studied, using X-ray diffraction and Mössbauer and magnetic measurements. These results have been compared to a more general theoretical study, on Zn_xCu_1−xFe₂O₄, based on mean field theory and high-temperature series expansions (HTSE), and extrapolated with the Padé approximant method. The nearest neighbour super-exchange interactions for the intra-site and the inter-site of Zn_xCu_1−xFe₂O₄ spinel ferrites, in the range 0≤x≤1, have been computed using the probability approach, based on Mössbauer data. The Curie temperature T_C is calculated as a function of Zn concentration. The theoretical results obtained are in good agreement with the experimental results obtained by magnetic measurements.     

Magnetic characterization of the non centrosymmetric Ba3NbFe3Si2O14 langasite

The potential relevance of the Ba₃NbFe₃Si₂O₁₄ langasite in the field of multiferroism was investigated. Interesting properties were expected, in particular in view of the frustrating stacking of its magnetic Fe³⁺ cations into triangular planes of triangle units. We hereafter report results of specific heat and magnetic measurements, Mössbauer spectroscopy and neutron diffraction. A peculiar magnetic structure is found out at low temperature. The Fe³⁺ magnetic moments adopt a triangular 120° configuration within each triangle, which is in-phase propagated in each triangular plane and is helically modulated from plane to plane.     

Mössbauer spectroscopy studies of spin reorientations in amorphous and crystalline (Co0.2Fe0.8)72.5Si12.5B15 glass coated micro-wires

Thermo-gravimetric, differential scanning calorimetry and comprehensive ⁵⁷Fe Mössbauer spectroscopy studies of amorphous and crystalline ferromagnetic glass coated (Co_0.2Fe_0.8)_72.5Si_12.5B₁₅ micro-wires have been recorded. The Curie temperature of the amorphous phase is T_C(amorp) ∼730 K. The analysis of the Mössbauer spectra reveals that below 623 K the easy axis of the magnetization is axial-along the wires, and that a tangential or/and radial orientation occurs at higher temperatures. At 770 K, in the first 4 hours the Mössbauer spectrum exhibits a pure paramagnetic doublet. Crystallization and decomposition to predominantly α-Fe(Si) and Fe₂B occurs either by raising the temperature above 835 K or isothermally in time at lower temperatures. Annealing for a day at 770 K, leads to crystallization. In the crystalline material the magnetic moments have a complete random orientation. After cooling back to ambient temperature, both α-Fe(Si) and Fe₂B in the glass coated wire show pure axial magnetic orientation like in the original amorphous state. The observed spin reorientations are associated with changes in the stress induced by the glass coating.     

Structural study by X-ray diffraction and Mössbauer spectroscopy of a new synthetic iron phosphate: K4MgFe3(PO4)5

A new iron phosphate K₄MgFe₃(PO₄)₅ has been synthesized by the flux method and characterized by single-crystal X-ray diffraction and Mössbauer spectroscopy. It crystallizes in the tetragonal system with the space group and the unit cell parameters a=9.714(3) Å and c=9.494(5) Å. The crystal structure is of a new type. It exhibits a three-dimensional framework built up from corner-sharing MO₅ (M=0.75Fe+0.25Mg) trigonal bipyramids and PO₄ tetrahedra. The K⁺ ions are occupying large eight-sided tunnels running along c. A room temperature Mössbauer study confirmed the +3 valence state of iron and its five-coordination.     

Temperature-dependent Mössbauer and dielectric studies of Mg0.95Mn0.05Fe1.0Ti1.0O4

The effect of tetravalent Ti⁺⁴ substitution in Mg_0.95Mn_0.05Fe₂O₄ on its magnetic and electrical properties has been studied using X-ray diffraction, Mössbauer spectroscopy, isothermal dc magnetization and dielectric measurements. X-ray diffraction studies have shown the structural transformation from cubic to tetragonal with the Ti⁺⁴ substitution. The Mössbauer spectra of Mg_0.95Mn_0.05Fe_1.0Ti_1.0O₄ recorded in the temperature range 20-300 K shows the presence of the magnetic as well as quadrupole interactions. The isothermal hysteresis loop infers that the system exhibits a ferrimagnetic ordering at room temperature. The Zero-field-cooled (ZFC) and field-cooled (FC) magnetization studies support ferrimagnetic ordering of Mg_0.95Mn_0.05Fe_1.0Ti_1.0O₄ at room temperature. Signatures of ferroelectric transition have been observed in the temperature range 200-300 K from dielectric measurements. The observed magnetic and dielectric behaviour indicate that this material exhibits multiferroic behaviour.     

Magnetic and structural features of amorphous FeMo-based alloys

NANOPERM-type FeMoCuB alloys are studied using magnetic and Mössbauer measurements in the as-prepared amorphous state. It is shown that the Fe₇₆Mo₈Cu₁B₁₅ (A) and Fe₇₄Mo₈Cu₁B₁₇ (B) alloys exhibit the magnetic dipole and electrical quadrupole interactions well detected in the room-temperature Mössbauer spectra. The thermomagnetic measurements above the room temperature indicate a vanishing of the magnetic interactions at approximately 310 K (A) and at 340 K (B), respectively. The low-temperature DC magnetic measurements show an anomaly around 200 K which is also a boundary at which zero-field Mössbauer measurements of both samples reflect the gradual “vanishing” of the electrical quadrupole interactions and appearance of another magnetically ordered component. The Mössbauer measurements in the field of 4 MA/m yield a survival of quadrupole and an enhancement of magnetic dipole interactions.     

Synthesis and characterization of lithium ferrite by oxalate precursor route

Nanocrystalline lithium ferrite (LiFe₅O₈) powders have been synthesized by oxalate precursor route. The effects of Fe³⁺/Li⁺ mole ratio, and annealing temperature on the formation, crystalline size, morphology and magnetic properties were systematically studied. The Fe³⁺/Li⁺ mole ratio was controlled from 5 to 3.33 while the annealing temperature was controlled from 600 to 1100 °C. The resultant powders were investigated by differential thermal analyzer (DTA), X-ray diffractometer (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). DTA results showed that LiFe₅O₈ phase started to form at around 520 °C. XRD indicated that LiFe₅O₈ phase always contained α-Fe₂O₃ impurity and the hematite phase formation increased by increasing the annealing temperature ?850 °C for different Fe³⁺/Li⁺ mole ratios 5, 4.55 and 3.85. Moreover, lithium ferrite phase was formed with high conversion percentage at critical annealing temperature 750–800 °C. Single well crystalline LiFe₅O₈ phase was obtained at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperatures from 800 to 1000 °C. Maximum saturation magnetization (68.7 emu/g) was achieved for the formed lithium ferrite phase at Fe³⁺/Li⁺ mole ratio 3.33 and annealing temperature 1000 °C.     

Synthesis and laser patterning of Bi-doped Y3Fe5O12 crystals in germanosilicate glasses

New germanosilicate glasses giving the crystallization of yttrium iron garnet Y₃Fe₅O₁₂ (YIG) and Bi-doped YIG, 23Na₂O-xBi₂O₃-(12−x)Y₂O₃-25Fe₂O₃-20SiO₂-20GeO₂ (mol%), are developed, and the laser-induced crystallization technique is applied to the glasses to pattern YIG and Bi-doped YIG crystals on the glass surface. It is clarified from the Mössbauer effect measurements that iron ions in the glasses are present mainly as Fe³⁺. It is suggested from the X-ray diffraction analyses and magnetization measurements that Si⁴⁺ ions are incorporated into YIG crystals formed in the crystallization of glasses. The irradiations (laser power: 32-60 mW and laser scanning speed: 7 μm/s) of continuous wave Yb:YVO₄ fiber laser (wavelength: 1080 nm) are found to induce YIG and Bi-doped YIG crystals, indicating that Fe³⁺ ions in the glasses act as suitable transition metal ions for the laser-induced crystallization. It is suggested that YIG and Bi-doped YIG crystals in the laser irradiated part might orient. The present study will be a first step for the patterning of magnetic crystals containing iron ions in glasses.     

Magnetic properties of RE0.7Ca0.3Mn0.95Fe0.05O3 (RE=Sm and Gd) manganites at low temperature

The magnetic properties of RE_0.7Ca_0.3Mn_0.95Fe_0.05O₃ perovskite with rare-earth cations (RE=Sm and Gd) were investigated by means of X-ray diffraction, Mössbauer spectroscopy, and low temperature (4.2-266 K) magnetization measurements. Structural characterization of these compounds shows that they both have orthorhombic (Pbnm) structure. The Mössbauer spectra show clear evidence of local structural distortion of the Mn(Fe)O₆ octahedron, which is based on the non-zero nuclear quadrupole interactions for high-spin Fe³⁺ ions. It was found that the local structural distortion increases significantly when Sm³⁺ is replaced by Gd³⁺. This distortion is attributed to the Jahn-Teller coupling strength as estimated from the Mössbauer effect results. The magnetic results indicate that the Curie temperature decreases as a result of replacing Sm by Gd. This is due to the decrease of the average A-site cationic radius 〈r_A〉. The rapid increase of magnetization at low temperature indicates the magnetic ordering of rare earth ions at the A-site.     

Heat-induced charge transfer in cobalt iron cyanide

The heating of Co(2+) ferricyanide above 80 °C induces an inner charge transfer from Co(2+) towards Fe(III) to form the mixed valence system Co(2+)Co(III) ferri- ferro-cyanide. This charge transfer takes place preserving the material framework and forming a solid solution of the initial and final species. The cell edge of the cubic cell (Fm-3m) of this solid solution follows a regular variation with the material composition. This mixed valence system was characterized using X-ray diffraction, infrared, thermo-gravimetric, Mössbauer and magnetic measurements. Its formation is easily detected by the appearance of an intermediate ν(CN) absorption band in the infrared spectra at around 2120 cm⁻¹, 40 cm⁻¹ below and above the observed frequency for this vibration in Co(2+) ferri- and ferro-cyanide, respectively.     

Mössbauer spectroscopy and magnetic properties in thin films of FexNi100−x electroplated on silicon (1 0 0)

Fe_xNi_100−x thin films were produced by galvanostatic electrodeposition on Si (1 0 0), nominal thickness 2800 nm, and x ranging 7-20. The crystalline structure of the sample was determined by X-ray diffraction (XRD). The magnetic properties were investigated by vibration sample magnetometry (VSM) and room temperature ⁵⁷Fe Mössbauer spectroscopy. Conversion Electron Mössbauer spectroscopy (CEMS) in both film surfaces for the thick self-supported films showed that the magnetic moment direction is in the plane and conventional transmission (MS) that the directions are out of the plane films. The results were interpreted assuming a three-layer model where the external layer has in-plane magnetization and the internal one, out of plane magnetization.