Exchange bias and anomalous vertical shift of the hysteresis loops in milled Fe/MnO2 material

The present article reports studies on structural and magnetic properties of nanostructured Fe/MnO₂ materials prepared by mechanosynthesis method, with Fe to MnO₂ ratios of 20/80, 50/50 and 60/40. X-ray diffraction patterns indicate that the milled materials have crystalline grain size in the nanoscale region. Mössbauer spectra of the milled materials suggest the presence of two Fe phases for each sample: a nanocrystalline α$\mathrm{\alpha }$-Fe phase with a high degree of disorder/defects and small Fe-oxide particles. The magnetic hysteresis (M(H)$M(H)$) loops, measured at 4.2 K, after the samples were cooled from 300 K in ±10 kOe fields, show unexpected large shifts in both horizontal and vertical directions for the 20/80 sample, while only horizontal shift was detected in the samples with higher Fe concentration. The anomalous vertical shift of the M(H)$M(H)$ loop for the 20/80 sample, observed at low cooling field (10 kOe), is being associated with a large contribution from non-collinear magnetic structure of the particles surface. This surface magnetic contribution is strongly influenced by the field cooling magnitude. A simple model is proposed to interpret this result.     

Exchange bias and vertical shift in CoFe2O4 nanoparticles

Magnetic properties of core–shell cobalt ferrite nanoparticles prepared by co-precipitation route in the range 15–48 nm have been studied. It is shown that the coercivity follows non-monotonic size dependence and exhibits a peak at around 26 nm. Field-cooled magnetization exhibited both horizontal (exchange bias) and vertical shifts. The exchange bias is understood as originating at the interface between a surface region (with structural and spin disorder) and a core ferrimagnetic region. The dependence of the exchange bias and vertical shift on the particle size and cooling field is found to have significant differences. These differences are explained in the light of recent results that suggest that there is a variation of the pinning strength amongst the interface spins and the vertical shift is affected by the more strongly pinned uncompensated spins.     

Permeability-frequency spectra of (Fe1−xcox)73.5Cu1Nb3Si13.5B9 nanocrystalline alloys under different magnetic fields

Under various amplitude of AC magnetic fields domain wall motion is the main mechanism in the magnetization process. This includes domain wall bulging and domain wall displacing. In this paper complex permeability-frequency spectra of (Fe_1−xCo_x)_73.5Cu₁Nb₃Si_13.5B₉ (x=0,0.5$x=0,0.5$) nanocrystalline alloys were measured as a function of the AC magnetic field, ranging from 0.001 to 0.04 Oe. Obvious changes have been found in complex permeability spectra for alloy x=0$x=0$ with the change of the amplitude of AC magnetic field, but variation of AC magnetic field has little effect on complex permeability spectra for alloy x=0.5$x=0.5$. This is attributed to the increased pinning field after substitution of Fe with Co in Fe_73.5Cu₁Nb₃Si_13.5B₉ nanaocrystalline alloy.     

Ferromagnetic-to-antiferromagnetic transition in (Hf1−xTix)Fe2 intermetallic compounds induced by geometrical frustration of the Fe(2a) sites

The ferromagnetic-to-antiferromagnetic transition in the hexagonal (Hf_1−xTi_x)Fe₂ (0?x?1) intermetallic compounds has been investigated by ⁵⁷Fe Mössbauer spectroscopy. At 10 K, the transition occurs within rather narrow concentration limits, around x=0.55–0.65. We found that the key factor governing the unexpected quick change of the magnetic structure is the magnetic frustration of the Fe(2a) sites. The magnetic frustration is caused by the noncollinearity of the Fe(6h) magnetic sublattice. The noncollinearity arises from the rotation of the magnetic moments due to the competition between the ferromagnetic exchange interactions and the antiferromagnetic Fe(6h)–Ti–Fe(6h) interaction. In the compounds with x=0.4–0.6, the temperature transitions to the antiferromagnetic state are observed. As an example, the Hf_0.4Ti_0.6Fe₂ compound is completely antiferromagnetic above 200 K.     

Positive exchange bias in a Ni80Fe20/NixFe1−xO thin-film bilayer

We have measured positive exchange bias in a Ni₈₀Fe₂₀/Ni_xFe_1−xO thin-film nanocrystallite system. A series of solid solution Ni_xFe_1−xO 40 nm thick films capped with 25 nm thick Ni₈₀Fe₂₀ were deposited using a range of %O₂/Ar bombardment energies (i.e. End-Hall voltages). Proper tuning of the deposition conditions results in a Ni₈₀Fe₂₀/Ni_xFe_1−xO (30%O₂/Ar) based bilayer that exhibits a positive exchange bias loop shift of H_ex∼60 Oe at 150 K.     

Preparation and characterizations of SiO2-coated nanoparticles of Mn0.4Zn0.6Fe2O4

Core/shell nanoparticles consisting of a magnetic core of zinc-substituted manganese ferrite (Mn_0.4Zn_0.6Fe₂O₄) and a shell of silica (SiO₂) are prepared by a sol-gel method using tetraethyl orthosilicate (TEOS) as a precursor material for silica and salts of iron, manganese and zinc as the precursor of the ferrite. Three weight percentages of the shell materials of SiO₂ are used to prepare the coated nanoparticles. The X-ray diffractograms (XRD) of the coated and uncoated magnetic nanoparticles confirmed that the magnetic nanoparticles are in their mixed spinel phase in an amorphous matrix of silica. Particles sizes of the samples annealed at different temperatures are estimated from the width of the (3 1 1) line of the XRD pattern using the Debye-Sherrer equation. The information regarding the crystallographic structure together with the particles sizes extracted from the high-resolution transmission electron microscopy (HRTEM) of a few selected samples are in agreement with those obtained from the XRD. HRTEM observations revealed that particles are coated with silica. The calculated thickness is in agreement with that obtained from the HRTEM pictures. Hysteresis loops observed in the temperature range 300 down to 5 K and Mössbauer spectra at room temperature indicate superparamagnetic relaxation of the nanoparticles.     

Soft magnetic properties and giant magneto-impedance effect of Fe73.5−xCrxSi13.5B9Nb3Au1 (x=1–5) alloys

In this paper, the effect of microstructural and surface morphological developments on the soft magnetic properties and giant magneto-impedance (GMI) effect of Fe_73.5−xCr_xSi_13.5B₉Nb₃Au₁ (x=1, 2, 3, 4, 5) alloys was investigated. It was found that the Cr addition causes slight decrease in the mean grain size of α-Fe(Si) grains. AFM results indicated a large variation of surface morphology of density and size of protrusions along the ribbon plane due to structural changes caused by thermal treatments with increasing Cr content. Ultrasoft magnetic properties such as the increase of magnetic permeability and the decrease of coercivity were observed in the samples annealed at 540 °C for 30 min. Accordingly, the GMI effect was also observed in the annealed samples.     

Structural and magnetic properties of Co1−xZnxFe2O4 nanoparticles by co-precipitation method

Co_1−xZn_xFe₂O₄ nanoparticles were prepared by co-precipitation method with x varying from 0 to 1.0. The powder samples were characterized by X-ray diffraction (XRD), vibrating sample magnetometer (VSM) and Fourier transform infrared spectroscopy (FTIR). The average crystallite sizes of the particles were determined from XRD. X-ray analysis showed that the samples were cubic spinel. The average crystallite size (D_aveXR) of the particles precipitated was found to vary from 6.92 to 12.02 nm decreasing with the increase in zinc substitution. The lattice constant (a_o) increased with the increase in zinc substitution. The specific saturation magnetization (M_S) of the particles was measured at room temperature. The magnetic parameters such as M_S, H_c, and M_r were found to decrease with the increase in zinc substitution. FTIR spectra of the Co_1−xZn_xFe₂O₄ with x varying from 0 to 1.0 in the range 400–4000 cm⁻¹ were reported. The spinel structure and the crystalline water adsorption of Co_1−xZn_xFe₂O₄ nanoparticles were studied by using FTIR.     

Solid state reaction synthesis of NiFe2O4 nanoparticles

Ni-ferrite (NiFe₂O₄) nanoparticles have been synthesized via a solid state reaction process. Ni and Fe bi-metallic nanoparticles in the form of Ni₃₃Fe₆₇ alloy nanopowder are first synthesized by simultaneous evaporation of the required amounts of pure Ni and Fe metals followed by rapid condensation of the evaporated metal flux into solid state by means of an inert gas, helium, using the process of inert gas condensation (IGC). In order to form the NiFe₂O₄ structure, as-synthesized samples (Ni₃₃Fe₆₇) are annealed for 12 h in ambient conditions at different annealing temperatures. Structural analyses show that NiFe₂O₄ starts to form at around 450 °C and gets progressively well defined with increasing annealing temperatures yielding particle with size ranging between 15 and 50 nm. Besides successfully forming NiFe₂O₄, NiO/Fe₃O₄ core/shell nanoparticles have also been synthesized by adjusting the annealing conditions. Three different structures, Ni₃₃Fe₆₇, NiO/Fe₃O₄, and NiFe₂O₄, obtained in this study are compared with respect to their structural and magnetic properties.     

Structure and magnetic properties of (Nd,Dy)16(Fe,Co)76−xTixB8 powders prepared by mechanical alloying

Nanocrystalline (Nd,Dy)₁₆(Fe,Co)_76−xTi_xB₈ magnets were prepared by mechanical alloying and respective heat treatment at 973–1073 K/30–60 min. An addition of 0.5 at % of Ti results in an increase of coercivity from 796 to 1115 kA m⁻¹. Partial substitution of Nd by Dy results in an additional increase of coercivity up to 1234 kA m⁻¹. Mössbauer investigations shows that for x?1 the (Nd,Dy)₁₆(Fe,Co)_76−xTi_xB₈ powders are single phase. For higher Ti contents (x>1) the mechanically alloyed powders heat treated at 973 K are no more single phase, and the coercivity decreases due to the presence of an amorphous phase. A heat treatment at a higher temperature (1073 K) for longer time (1 h) results in the full recrystallisation of powders. The mean hyperfine field of the Nd₂Fe₁₄B phase decreases for titanium contents of 0?x?1, and remains constant for x>1. This indicates that the Ti content in the Nd₂Fe₁₄B phase reaches its maximum value.     

Mössbauer studies on the superparamagnetic behavior of CoFe2O4 with a few nanometers

CoFe₂O₄ nanoparticles with a cubic spinel structure are prepared by a high-temperature thermal decomposition method. The average particle sizes are 4.6  and 5.7 nm for CoFe₂O₄ made with two kinds of solvents by TEM. Mössbauer spectra of 4.6 nm particles displayed a superparamagnetic behavior as demonstrated by a single line with zero hyperfine fields, but that of 5.7 nm particles did not at room temperature. It is considered that anisotropy energy was still more superior to thermal energy because of particle size of 5.7 nm CoFe₂O₄. Furthermore, Mössbauer spectra exhibited the typical spectrum shapes of the CoFe₂O₄ at 4.2 K. The spectrum at 4.2 K was fitted using two magnetic components of hyperfine fields _Hhf=540.4,512.6$H_{\mathrm{hf}}=540.4,512.6$ kOe and isomer shifts δ=0.40,0.30$\delta =0.40,0.30$ mm/s for 4.6 nm and _Hhf=542.7,512.8$H_{\mathrm{hf}}=542.7,512.8$ kOe and δ=0.41,0.29$\delta =0.41,0.29$ mm/s for 5.7 nm corresponding to Fe³⁺ ions at site A and site B, respectively.     

Fabrication and magnetic properties of Fe3O4 nanowire arrays in different diameters

Fe₃O₄ nanowire arrays with different diameters of D=50, 100, 150 and 200 nm were prepared in anodic aluminum oxide (AAO) templates by an electrodeposition method followed by heat-treating processes. A vibrating sample magnetometer (VSM) and a Quantum Design SQUID MPMS magnetometer were used to investigate the magnetic properties. At room temperature the nanowire arrays change from superparamagnetism to ferromagnetism as the diameter increases from 50 to 200 nm. The zero-field-cooled (ZFC) and field-cooled (FC) magnetization measurements show that the blocking temperature T_B increases with the diameter of nanowire. The ZFC curves of D=50 nm nanowire arrays under different applied fields (H) were measured and a power relationship between T_B and H were found. The temperature dependence of coercivity below T_B was also investigated. Mössbauer spectra and micromagnetic simulation were used to study the micro-magnetic structure of nanowire arrays and the static distribution of magnetic moments of D=200 nm nanowire arrays was investigated. The unique magnetic behaviors were interpreted by the competition of the demagnetization energy of quasi-one-dimensional nanostructures and the magnetocrystalline anisotropy energy of particles in nanowires.     

Synthesis and magnetic properties of CoFe2O4 ferrite nanoparticles

CoFe₂O₄ ferrite nanoparticles were prepared by a modified chemical coprecipitation route. Structural and magnetic properties were systematically investigated. X-ray diffraction results showed that the sample was in single phase with the space group . The results of field-emission scanning electronic microscopy showed that the grains appeared spherical with diameters ranging from 20 to 30 nm. The composition determined by energy-dispersive spectroscopy was stoichiometry of CoFe₂O₄. The Curie temperature in the process of increasing temperature was slightly higher than that in the process of decreasing temperature. This can be understood by the fact that heating changed Co²⁺ ion redistribution in tetrahedral and in octahedral sites. The coercivity of the synthesized CoFe₂O₄ samples was lower than the theoretical values, which could be explained by the mono-domain structure and a transformation from ferrimagnetic to superparamagnetic state.     

Magnetic properties of nanocrystalline Co1−xZnxFe2O4 prepared by forced hydrolysis method

Nanocrystalline zinc-substituted cobalt ferrite powders, Co_1−xZn_xFe₂O₄ (x=0, 0.2, 0.4), were for the first time prepared by forced hydrolysis method. Magnetic and structural properties in these specimens were investigated. The average crystallite size is about 3.0 nm. When the zinc substitution increases from x=0 to x=0.4, at 4.2 K, the saturation magnetization increases from 72.1 to 99.7 emu/g and the coercive field decreases from 1.22 to 0.71 T. All samples are superparamagnetic at room temperature and ferrimagnetic at temperatures below the blocking temperature. The high value of the saturation magnetization and the very thin thickness of the disorder surface layer of all samples suggests that this forced hydrolysis method is suitable not only for preparing two metal element systems but also for three or more ones.     

Morphology and magnetic properties of Co0.8Fe2.2O4 films prepared by the chemical solution deposition

Co_0.8Fe_2.2O₄ ferrite thin films have been prepared on Si(0 0 1) substrates by the chemical solution deposition. Structural characteristics indicate all films are single phase with spinel structure and the space group and the mean grain size increases from 8 to 30 nm with the increase of annealing temperature. The magnetic properties of Co_0.8Fe_2.2O₄ thin films are highly dependent on annealing temperature. The sample annealed at 800 °C possesses high saturation magnetization, moderate coercivity and squareness ratio, making it a promising application candidate in high-density record and magneto-optical materials.     

Crystal structure and magnetic properties of RCu5−xPdx (R=Pr, Nd, Sm and Eu) alloys

We report the effect of replacing Cu by Pd in RCu₅ (R=Pr, Nd, Sm and Eu). The parent RCu₅ compounds crystallize in the hexagonal CaCu₅-type structure. The hexagonal symmetry is retained in PrCu₄Pd and EuCu_5−xPd_x (x=1 and 2) but the crystal structure changes to cubic AuBe₅-type in PrCu₃Pd₂, NdCu_5−xPd_x (x=1 and 2) and SmCu₄Pd. Substitution with Pd leads to lattice expansion and modifies the magnetic behavior. While PrCu₅ is known to be a van-Vleck paramagnet with a singlet ground state, PrCu₄Pd and PrCu₃Pd₂ show ferromagnetic-like behavior at low temperatures. SmCu₄Pd orders ferromagnetically near 28 K in contrast to the antiferromagnetic nature of the parent SmCu₅. The divalent nature of the Eu ions in EuCu₅ is retained in the ternary alloys, but the Curie temperature is reduced from 57 to 24.5 and 14.5 K in EuCu₄Pd and EuCu₃Pd₂, respectively, inferred from the location of peak in the heat capacity of these two compounds. The magnetic hyperfine field at the Eu nucleus measured with ¹⁵¹Eu Mössbauer spectroscopy in the ternary Eu-alloys is comparable to that in EuCu₅. The magnetic behavior of NdCu₄Pd is similar to that reported in NdCu₅. The zero-field-cooled, low-field magnetization of NdCu₃Pd₂ shows a region of diamagnetic behavior roughly between 21 and 4 K, but the field-cooled response is positive.     

Effect of carbon content on structure and magnetic properties for (Fe,Ni)1−xCx by mechanical alloying

FCC (Fe₅₅Ni₄₅)_1−xC_x   supersaturated solid solution was prepared in a wide concentration range (0?x?0.9)$(0?x?0.9)$ by mechanical alloying of nanocrystalline Fe₅₅Ni₄₅ with graphite. The lattice constant of Fe₅₅Ni₄₅ increases linearly with increasing carbon content up to x=0.25$x=0.25$. At the same time, it is found that the magnetic moment per metal atom (Fe, Ni) decreases linearly with increasing carbon content for 0?x?0.25$0?x?0.25$ with a slope of 1.2 μ_B/at. For high carbon content, x?0.5$x?0.5$, it is observed that the decrease of lattice constant and increase of moment per metal atom (Fe, Ni) with increasing C content, indicates that the dissolution of carbon is hindered by the high-volume fraction of graphite in the initial powder mixture. The complete amorphization of x=0.5$x=0.5$ does not occur after the extended ball milling. The alloying effect of carbon on the magnetization is compared with other metalloid B, P, and Si in Fe- and Ni-based binary system.     

Phase boundary between uniaxial and planar ferromagnets in layered perovskite manganite La2−2xSr1+2xMn2O7 (0.313⩽x⩽0.350)

We have examined magnetizations as a function of temperature and magnetic field in layered perovskite manganites La_2−2xSr_1+2xMn₂O₇ single crystals (x=0.313, 0.315, 0.318, 0.320 and 0.350) in order to determine the phase boundary between two ferromagnets (one is an uniaxial ferromagnet whose easy axis is parallel to the c-axis and the other is a planar ferromagnet whose easy axis is within the ab-plane) and following results are obtained: (i) all the present manganites exhibit magnetic transitions from a ferromagnet to a paramagnet at 76, 107, 116, 120 and 125 K for x=0.313, 0.315, 0.318, 0.320 and 0.350, respectively; (ii) for x=0.318, 0.320 and 0.350, the magnetic structure is a planar ferromagnet below Curie temperature; (iii) for x=0.313 and 0.315, the magnetic structure changes from an uniaxial to a planar ferromagnet at 66 and 85 K, respectively. From the results described above we have constructed the magnetic phase diagram of layered perovskite manganite La_2−2xSr_1+2xMn₂O₇ (0.313?x?0.350).     

The exchange bias in MnPd/Co1−xFex bilayers

A systematic study of exchange bias in MnPd/Co and MnPd/Co_1−xFe_x bilayers has been carried out. Very large unidirectional anisotropy constant of 2.2 erg/cm² and the appearance of double-shifted loops, ascribed to the coexistence of positive and negative exchange bias, have been observed. The dependence of exchange bias, unidirectional anisotropy constant and coercivity on thickness, temperature, annealing regime and Fe content has been investigated and discussed.     

Numerical simulation of magnetic interactions in polycrystalline YFeO3

The magnetic behavior of polycrystalline yttrium orthoferrite was studied from the experimental and theoretical points of view. Magnetization measurements up to 170 kOe were carried out on a single-phase YFeO₃ sample synthesized from heterobimetallic alkoxides. The complex interplay between weak-ferromagnetic and antiferromagnetic interactions, observed in the experimental M(H) curves, was successfully simulated by locally minimizing the magnetic energy of two interacting Fe sublattices. The resulting values of exchange field (H_E=5590 kOe), anisotropy field (H_A=0.5 kOe) and Dzyaloshinsky–Moriya antisymmetric field (H_D=149 kOe) are in good agreement with previous reports on this system.