Evolution of magnetic order in mechanically alloyed Al–1 at%Fe

The evolution of ferromagnetic order in high-energy ball-milled Al–1 at% Fe before the onset of a considerable Fe–Al solid solution phase has been investigated using ⁵⁷Fe Mössbauer and bulk magnetization studies. The unmilled sample does not exhibit bulk magnetic properties and an onset of bulk magnetization is observed only after 30 min of milling, when the grain size becomes comparable to the ferromagnetic exchange length. The Curie temperatures of all the samples are less than that of pure iron. The reduction in grain size is accompanied by an increase in coercivity and reduced remanence and a decrease in T_C. The effective magnetic moment per iron atom decreases with the development of a non-magnetic, Al-rich Fe–Al solution on longer milling. The clustering of Fe at grain boundaries is responsible for the observed bulk magnetic ordering. The systematic variation of the magnetic properties has been qualitatively correlated with the evolution of microstructure, reduction in grain size and enhanced inter-granular exchange coupling.     

Magnetic and structural studies of mechanically alloyed nanostructured Fe49Co49V2 powders

Nanostructured Fe₄₉Co₄₉V₂ powders were produced by high energy milling at different milling times and then examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The saturation magnetization and coercivity of samples were measured at room temperature by a vibration sample magnetometer (VSM). Structural studies show that as the milling time increases from 0 to 125 h, the average grain size reduces from 130 to about 8-10 nm, while the microstrain increases up to 1.7%. The lattice parameter decreases from 0 to 36 h and then increases up to 125 h. According to the XRD patterns, the formation of intermetallic compound of (Fe, Co)V after about 16 h affects the magnetic properties. The coercivity totally increases up to 61 Oe due to the introduction of microstrain during the milling process. Magnetic measurements reveal that the saturation magnetization has some fluctuations during the milling treatment and finally at 125 h reaches about 180 emu/g     

Finite size effects on the structural and magnetic properties of sol–gel synthesized NiFe2O4 powders

Nanoparticles of nickel ferrite have been synthesized by the sol–gel method and the effect of grain size on its structural and magnetic properties have been studied in detail. X-ray diffraction (XRD) studies revealed that all the samples are single phasic possessing the inverse spinel structure. Grain size of the sol–gel synthesized powders has been determined from the XRD data and the strain graph. A grain size of 9 nm was observed for the as prepared powders of NiFe₂O₄ obtained through the sol–gel method. It was also observed that strain was induced during the firing process. Magnetization measurements have been carried out on all the samples prepared in the present series. It was found that the specific magnetization of the nanosized NiFe₂O₄ powders was lower than that of the corresponding coarse-grained counterparts and decreased with a decrease in grain size. The coercivity of the sol–gel synthesized NiFe₂O₄ nanoparticles attained a maximum value when the grain size was 15 nm and then decreased as the grain size was increased further.     

Effect of aluminum substitution on the structural and magnetic properties of cobalt ferrite synthesized by sol-gel auto combustion process

Aluminum substituted cobalt ferrite powders (CoFe_2−xAl_xO₄) with varying composition from 0.0 to 1.0 in the step of 0.2 have been obtained by sol-gel auto combustion technique using citric acid as a fuel. The metal nitrate to fuel ratio was maintained 1:4 throughout the synthesis of CoFe_2−xAl_xO₄. The thermal analysis of as prepared samples is done by TGA technique. The compositional stoichiometry of the prepared samples is confirmed by Energy dispersive X-ray analysis technique. Single phase cubic spinel structure and nano phase structure of the synthesized powders were confirmed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystallite size of 16-26 nm was obtained using Scherrer formula. SEM analysis shows the formation of uniform grain growth. The grain size obtained from SEM results is of the order of 30 nm. Maximum specific surface area was observed to be of the order of 52 m²/gm. The highest value of saturation magnetization and coercivity was observed for pure cobalt ferrite sample and it decreases as the aluminum content x increases. A strong co-relation between the saturation magnetization and aluminum content was observed. The decrease in magnetic properties is due to the substitution of aluminum ions in place of Fe³⁺.     

Investigation of magnetic properties of Al substituted nickel ferrite nanopowders, synthesized by the sol-gel method

NiFe_2−xAl_xO₄ nanopowders, where x is from 0 to 1.5 with a step of 0.5, have been synthesized by the sol-gel method and the effect of non-magnetic aluminum content on their structural and magnetic properties were investigated. The X-ray diffraction (XRD) patterns revealed that the synthesized nanopowders are single phase with a spinel structure. Mean crystallite sizes of the samples were calculated by Scherrer's formula and were in the range 20-31 nm. The morphology of the nanopowders was investigated by TEM and the mean particle sizes of the samples were in the range 55-80 nm. Magnetic hysteresis loops were recorded at room temperature in a maximum applied field of 3000 Oe. The results show that by increasing the aluminum content, the magnetizations of the nanopowders are decreased. This reduction is caused by non-magnetic Al³⁺ ions, which by their substitutions the super exchange interactions between different sites will be reduced. It is also seen that the magnetizations of the nanopowders are lower than those related to their bulk counterparts. This reduction was found to be as a consequence of surface spin disorder. M-T curves of the samples were obtained using a Faraday balance and by which the Curie temperatures of the powders were determined. The results that are obtained show that the Curie temperatures of the nanopowders are higher than those of their bulk counterparts.     

Sol-gel derived nanoparticles of Zn substituted lithium ferrite (Li0.32Zn0.36Fe2.32O4): magnetic and Mössbauer effect measurements and their theoretical analysis

Nanoparticles of Zn substituted lithium ferrite (Li_0.32Zn_0.36Fe_2.32O₄) have been prepared by a sol-gel method where the ultra-sonication technique has been adopted to reduce the agglomeration effect among the nanoparticles. The samples were heat-treated at three different temperatures and the formation of the nanocrystalline phase was confirmed by X-ray diffractograms (XRD). The average particle size of each sample has been estimated from the (311) peak of the XRD pattern using the Debye-Scherrer formula and the average sizes are in the range of 10-21 nm. The average particle size, crystallographic phase, etc. of some selected samples obtained from the high-resolution transmission electron microscopy are in agreement with those estimated from the XRD patterns. Static magnetic measurements viz., hysteresis loops, field cooled and zero field cooled magnetization versus temperature curves of some samples carried out by SQUID in the temperature range of 300 to 5 K clearly indicate the presence of superparamagnetic (SPM) relaxation of the nanoparticles in the samples. The maximum magnetization of the SPM sample annealed at 500 °C is quite high (68 Am²/Kg) and the hysteresis loops are almost square shaped with very low value of coercive field at room temperature (827.8 A/m). The particle size, magneto-crystalline anisotropy, etc. have been estimated from the detailed theoretical analysis of the static magnetic data. The dynamic magnetic behavior of the samples was also investigated by observing the ac hysteresis loops and magnetization versus field curves with different time windows at room temperatures. The different soft magnetic quantities viz., coercive field, magnetization, remanance, hysteresis losses, etc. were extracted from dynamic measurements. Dynamic measurements confirmed that the samples are in their mixed state of SPM and ordered ferrimagnetic particles, which is in good agreement with the results of static magnetic measurements. Mössbauer spectra of the samples recorded at room temperature (300 K) and at different temperatures down to 20 K confirmed the presence of the SPM relaxation of the nanoparticles of the samples.     

Phase formation and change of magnetic properties in mechanical alloyed Ni0.5Co0.5Fe2O4 by annealing

The effects of milling time and annealing temperature on phase formation, microstructure and magnetic properties of nickel-cobalt ferrite synthesized from oxide precursors by mechanical alloying were studied. The study of milling time effects on phase formation of milled materials showed that if milling continues up to 55 h, single phase nano-sized nickel-cobalt ferrite is obtained. Also, magnetic properties of powders versus milling time and annealing at different temperatures extensively changed, so that annealing at 1200 °C increased the magnetization saturation of the as-milled powder from 15.1 to 53.6 emu/g. X-ray powder diffraction technique (XRD) with Cu-Ka radiation was employed for phase identification. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were also used to determine the morphology and size of the particles. The magnetic properties were measured by a vibration sample magnetometer (VSM).     

Preparation and properties of nanocrystalline powders in (Y1−xCex)3Al5O12 system

Nano-sized cerium-doped yttrium aluminum garnet (YAG:Ce) phosphors were synthesized via a simple sol-gel process using metal nitrate precursors. The prepared phosphors were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy, respectively. Pure cubic garnet phase was formed at temperatures ∼900 ^οC. The particle sizes of as-prepared powders were mostly in the range of 17-27 nm. The crystalline YAG:Ce showed broad emission peaks in the range of 400-700 nm and maximum intensities at 500 and 520 nm. It is found also that the emission intensity decreased with increasing Ce doping concentration from 0.1 to 1.5 at%. With increasing Ce doping concentration, the PL intensity was shifted towards shorter wavelengths.     

Magnetic properties of xNi0.53Cu0.12Zn0.35Fe1.88O4+(1−x)BaTiO3 nanocomposites

The nanocrystalline Ni_0.53Cu_0.12Zn_0.35Fe_1.88O₄ and BaTiO₃ powders were prepared using Microwave-Hydrothermal (M-H) method at 160 °C/45 min. The as synthesized powders were characterized using the X-ray diffraction (XRD) and Transmission Electron Microscope (TEM). The size of the powders that were synthesized using M-H system was found to be ∼30 and ∼50 nm for ferrite phase and ferroelectric phases, respectively. The powders were densified using microwave sintering method at 900 °C/30 min. The ferrite and ferroelectric phases were observed from XRD and morphology of the composites was observed with the Scanning Electron Microscope (SEM).The magnetic hysteresis loops were recorded using the Vibrating Sample Magnetometer (VSM).The frequency dependence of real (μ′) and imaginary (μ″) parts of permeability was measured in the range of 1 MHz-1.8 GHz. The permeability decreases with an increase of BaTiO₃ content at 1 MHz. The transition temperature (T_C) of ferrite was found to be 245 °C. The T_C of composite materials decreases with an increase in BaTiO₃ content.     

Magnetic properties of electron-doped Y1−xCexMnO3 compounds

Cerium-doped Y_1−xCe_xMnO₃ compounds have been prepared in single-phase form for x=0 to 0.10. X-ray diffraction (XRD) patterns could be analyzed by using P6₃cm space group. Temperature variations of ac susceptibility and magnetization measurements show that these Ce-doped materials exhibit weak ferromagnetic transition. The observed ferromagnetic transition is attributed to the double exchange ferromagnetic interaction between Mn²⁺ and Mn³⁺ ions due to electron doping. The M–H loops exhibit hysteresis along with linear contribution and were analyzed based on bound magnetic polaron (BMP) model. Increase in saturation magnetization and decrease in BMP concentrations have been observed with increase in Ce doping.     

The effect of La-substitution on magnetic properties of nanosized Sr1−xLaxTi0.05Zn0.2(Fe)11.75−δ(Fe)δO19 powders

A series of La-substituted M-type Sr hexaferrite powders Sr_1−xLa_xTi_0.05Zn_0.2Fe³⁺_11.75O₁₉, wherein x ranges from 0.1 to 0.5 with a step of 0.1, have been prepared by the conventional ceramic method and were then milled in a high energy mill to prepare nanosized powders. XRD investigation of the calcined and the milled powders shows that single phase hexaferrite structure has been formed after calcining and has not changed after milling. The lattice parameters and the mean crystallite sizes of the samples have been determined from the XRD data and Scherrer's formula. The results show that the lattice parameters (“а” and “c”) decrease with increase in La-substitution and the mean crystallite size of the milled powders is about 17 nm. Coercivities and magnetizations of the samples in a magnetic field of 16 kOe have been determined from the room temperature hysteresis loops. It was found that both parameters increase with La substitutions up to 0.3 and then decrease for higher substitutions. These variations were attributed to the enhancement of hyperfine field and spin-canting magnetic structure when La content increases. In addition, the magnetizations were smaller for the nanosized samples in comparison with those of bulk ones, which were discussed according to the core-shell model. Also the results show that annealing of the nanosized samples up to 500 °C can enhance coercivity and magnetization of the samples, which is discussed based on crystallite size growth.     

Monodispersed nanocrystalline Co1–xZnxFe2O4 particles by forced hydrolysis: Synthesis and characterization

Zinc-substituted cobalt ferrites, Co_1–xZn_xFe₂O₄, were for the first time successfully prepared by forced hydrolysis method. The obtained materials are single phase, monodispersed nanocrystalline with an average grain size of about 3 nm. These materials are superparamagnetic at room temperature and ferrimagnetic at temperature lower than the blocking temperature. When the zinc substitution increases from x=0 to 0.4, at 4.2 K, the saturation magnetization increases from 72.1 to 99.7 emu/g. The high saturation magnetization of these samples suggests that this method is suitable for preparing high-quality nanocrystalline magnetic ferrites for practical applications.     

Magnetocaloric effect in high-energy ball-milled Gd5Si2Ge2 and Gd5Si2Ge2/Fe nanopowders

Evolution of structure and magnetocaloric properties in ball-milled Gd₅Si₂Ge₂ and Gd₅Si₂Ge₂/0.1 wt% Fe nanostructured powders were investigated. The high-energy ball-milled powders were composed of very fine grains (70–80 nm). Magnetization decreased with milling time due to decrease in the grain size and randomization of the magnetic moments at the surface. The magnetic entropy change (ΔS_M) was calculated from the isothermal magnetization curves and a maximum value of 0.45 J/kg K was obtained for 32 h milled Gd₅Si₂Ge₂ alloy powder for a magnetic field change of 2 T while it was still low in Fe-contained alloy powders. The thermo-magnetic measurements revealed that the milled powders display distribution of magnetic transitions, which is desirable for practical magnetic refrigerant to cover a wide temperature span.     

Structural and magnetic properties of sol-gel Co2xNi0.5−x Zn0.5−xFe2O4 thin films

Nanocrystalline Co_2xNi_0.5−xZn_0.5−xFe₂O₄ (x=0−0.5) thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology as well as magnetic and microwave absorption properties of the films calcined at 1073 K were studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. All films were uniform without microcracks. The Co content in the Co-Ni-Zn films resulted in a grain size ranging from 15 to 32 nm while it ranged from 33 to 49 nm in the corresponding powders. Saturation and remnant magnetization increased with increase in grain size, while coercivity demonstrated a drop due to multidomain behavior of crystallites for a given value of x. Saturation magnetization increased and remnant magnetization had a maximum as a function of grain size independent of x. In turn, coercivity increased with x independent of grain size. Complex permittivity of the Co-Ni-Zn ferrite films was measured in the frequency range 2-15 GHz. The highest hysteretic heating rate in the temperature range 315-355 K was observed in CoFe₂O₄. The maximum absorption band shifted from 13 to 11 GHz as cobalt content increased from x=0.1 to 0.2.     

Synthesis and magnetic characterization of Zn0.6Ni0.4Fe2O4 nanoparticles via a polyethylene glycol-assisted hydrothermal route

Zn-doped nickel ferrite nanoparticles (Zn_0.6Ni_0.4Fe₂O₄) have been prepared via a surfactant, polyethylene glycol assisted hydrothermal route. X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy, transmission electron microscopy (TEM), and vibrating scanning magnetometry (VSM) were used for the structural, morphological, and magnetic characterizations of the product, respectively. TEM analysis revealed that the nanoparticles have a narrow size distribution, with average particle size of 15±1 nm, which agrees well with the XRD based estimate of 14±2 nm. The absence of saturation and remanent magnetization, and coercivity in the high temperature region of the M-H curve and non-zero magnetic moments indicate superparamagnetism of the nanoparticles with a canted spin structure. The appearance of a peak on the temperature-dependent zero-field cooling magnetization curve at ∼190 K indicates the blocking temperature of the sample.     

Influence of milling time on the structural, microstructural and magnetic properties of mechanically alloyed Ni58Fe12Zr10Hf10B10 nanostructured/amorphous powders

This paper investigates structural, microstructural and magnetic properties of amorphous/nanocrystalline Ni₅₈Fe₁₂Zr₁₀Hf₁₀B₁₀ powders prepared by high energy milling. Ball milling of Ni, Fe, Zr, Hf and B leads to alloying of the element powders at 120 h. The results show that at 190 h the amorphous content is at the highest level and the grain size is about 2 nm. The magnetic measurements reveal that the coercivity and the saturation magnetization reach about 20 Oe and 30 emu/g at 190 h and become approximately 5 Oe and 40 emu/g after a suitable heat treatment, respectively.     

Growth temperature dependence of the hysteretic behavior of Ni0.5Zn0.5Fe2O4 thin films

Herein, a discussion of the effect of deposition temperature on the magnetic behavior of Ni_0.5Zn_0.5Fe₂O₄ thin films. The thin films were grown by r.f. sputtering technique on (1 0 0) MgO single-crystal substrates at deposition temperatures ranging between 400 and 800 °C. The grain boundary microstructure was analyzed via atomic force microscopy (AFM). AFM images show that grain size (φ∼70-112 nm) increases with increasing deposition temperature, according to a diffusion growth model. From magneto-optical Kerr effect (MOKE) measurements at room temperature, coercive fields, H_c, between 37and 131 Oe were measured. The coercive field, H_c, as a function of grain size, reaches a maximum value of 131 Oe for φ ∼93 nm, while the relative saturation magnetization exhibits a minimum value at this grain size. The behaviors observed were interpreted as the existence of a critical size for the transition from single- to multi-domain regime. The saturation magnetization (21 emu/g<M_s<60 emu/g) was employed to quantify the critical magnetic intergranular correlation length (L_c≈166 nm), where a single-grain to coupled-grain behavior transition occurs. Experimental hysteresis loops were fitted by the Jiles-Atherton model (JAM). The value of the k-parameter of the JAM fitted by means of this model (k/μ_o∼50 A m²) was correlated to the domain size from the behavior of k, we observed a maximum in the density of defects for the sample with φ∼93 nm.     

Structural and magnetic studies on mechanosynthesized BaFe12−xMnxO19

Barium hexaferrite powders with manganese substitution were prepared by mechanosynthesis. The structural and magnetic properties were characterized by X-ray diffractometer and vibration sample magnetometer, respectively. XRD patterns were refined by Rietveld method. Preferential site occupation of manganese ion was investigated by room temperature (RT) Mössbauer measurements. XRD results showed a single-phase barium hexaferrite with some residual hematite. Crystallite size was observed to decrease with substitution amount. Lower saturation magnetization and increased coercivity is observed in substituted samples. RT Mössbauer measurements showed that manganese ions preferentially occupy 12k, 4f₂, and 2a sites.     

Structural and magnetic properties of Mg(In2−xMnx)O4 system

We synthesized the Mn-doped Mg(In_2−xMn_x)O₄ oxides with 0.03?x?0.55 using a solid-state reaction method. The X-ray diffraction patterns of the samples were in a good agreement with that of a distorted orthorhombic spinel phase. Their lattice parameters and unit-cell volumes decrease with x due to the substitution of the smaller Mn³⁺ ions to the larger In³⁺ ions. The undoped MgIn₂O₄ oxide presents diamagnetic signals for 5 K?T?300 K. The M(H) at T=300 K reveals a fairly negative-sloped linear relationship. Neither magnetic hysteresis nor saturation behavior was observed in this parent sample. For the Mn-doped samples, however, positive magnetization were observed between 5 and 300 K even if the x value is as low as 0.03. The mass susceptibility enhances with Mn content and it reaches the highest value of 1.4×10⁻³ emu/g Oe (at T=300 K) at x=0.45. Furthermore, the Mn-doped oxides with x=0.06 and 0.2, respectively, exhibit nonlinear magnetization curves and small hysteretic loops in low magnetic fields. Susceptibilities of the Mn-doped samples are much higher than those of MnO₂, Mn₂O₃ oxides, and Mn metals. These results show that the oxides have potential to be magnetic semiconductors.     

XRD,magnetic and Mössbauer spectral studies of nano size aluminum substituted cobalt ferrites (CoAlxFe2−xO4)

Aluminum substituted cobalt ferrites having particle size ∼10 nm were prepared using aerosol route, which increases with annealing temperature. The unit cell parameter ‘a’ and saturation magnetization decreases linearly with the increase of aluminum concentration. This is due to the smaller ionic radius and the diamagnetic nature of the Al³⁺, respectively. Room temperature Mössbauer spectra of the samples annealed at 1200 °C show broad sextets, which were fitted with different sextets, indicating different local environment of both tetrahedrally and octahedrally coordinated iron cation. Further, hyperfine field of the samples decreases with the increase of Al³⁺ concentration due to the fact that the Al³⁺ diamagnetic species reduce the magnetic interactions. Cations distribution indicated a increase in Fe³⁺(oct.)/Fe³⁺(tet.) ratio on increasing the Al³⁺ concentration.