Synthesis and magnetic properties of NiFe2−xAlxO4 nanoparticles

Nanocrystalline Al-doped nickel ferrite powders have been synthesized by sol–gel auto-ignition method and the effect of non-magnetic aluminum content on the structural and magnetic properties has been studied. The X-ray diffraction (XRD) revealed that the powders obtained are single phase with inverse spinel structure. The calculated grain sizes from XRD data have been verified using transmission electron microscopy (TEM). TEM photographs show that the powders consist of nanometer-sized grains. It was observed that the characteristic grain size decreases from 29 to 6 nm as the non-magnetic Al content increases, which was attributed to the influence of non-magnetic Al concentration on the grain size. Magnetic hysteresis loops were measured at room temperature with a maximum applied magnetic field of ≈1 T. As aluminum content increases, the measured magnetic hysteresis curves become more and more narrow and the saturation magnetization and remanent magnetization both decreased. The reduction of magnetization compared to bulk is a consequence of spin non-collinearity. Further reduction of magnetization with increase of aluminum content is caused by non-magnetic Al³⁺ ions and weakened interaction between sublattices. This, as well as the decrease in hysteresis was understood in terms of the decrease in particle size.     

Study on electro-magnetic properties of La substituted Ni–Cu–Zn ferrite synthesized by auto-combustion method

(Ni_0.25Cu_0.20Zn_0.55)La_xFe_2−xO₄ ferrite with x=0.00, 0.025, 0.050 and 0.075 compositions were synthesized through nitrate–citrate auto-combustion method. Crystalline spinel ferrite phase with about 16–19 nm crystallite size was present in the as-burnt ferrite powder. These powders were calcined, compacted and sintered at 950 °C for 4 h. Initial permeability, magnetic loss and AC resistivity of different compositions were measured in the frequency range from 10 Hz to 10 MHz. Saturation magnetization and hysteresis parameters were measured at room temperature with a maximum magnetic field of 10 kOe. Permeability and AC resistivity were found to increase and magnetic loss decreased with La substitution for Fe, up to x=0.025. Saturation magnetization and coercive field also increases up to that limit. The electromagnetic properties were found best in the ferrite composition of x=0.025, which would be better for more miniaturized multi layer chip inductor.     

Investigating the magnetic properties of soft magnetic composites based on mechanically alloyed nanocrystalline Fe-5 wt% Ni powders

In this work, the soft magnetic composites (SMCs) of the nanocrystalline Fe-5 wt% Ni powders coated with phenolic resin were studied. The nanocrystalline powders with an average diameter of 10 nm were obtained by mechanical alloying up to 96 h milling in a high-energy planetary ball mill. The microstructure and magnetic properties of the milled powders were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy and a vibrating sample magnetometer. The results of X-ray diffraction showed that the bcc Fe(Ni) solid solution is formed after 24 h milling. Magnetic measurements indicated that the 96 h milled powders with a steady-state grain size of 10 nm have the highest saturation magnetization and the lowest coercivity. The SMCs based on nanocrystalline powders showed higher electrical resistivity and magnetic permeability up to 1 MHz, as compared with the pure iron-based composites. Besides, the nanocrystalline-based SMCs exhibited higher relaxation frequency and a significantly lower loss factor up to 1 MHz.     

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     

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).     

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.     

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.     

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.     

X-ray diffraction,microstructure, Mössbauer and magnetization studies of nanostructured Fe50Ni50 alloy prepared by mechanical alloying

Nanocrystalline Fe₅₀Ni₅₀ alloy samples were prepared by the mechanical alloying process using planetary high-energy ball mill. The alloy formation and different physical properties were investigated as a function of milling time, t, (in the 0–50 h range) by means of the X-ray diffraction (XRD) technique, scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), Mössbauer spectroscopy and the vibrating sample magnetometer (VSM). The complete formation of γ-FeNi is observed after 24 h milling. When milling time increases from 0 to 50 h, the lattice parameter increases towards the Fe₅₀Ni₅₀ bulk value, the grain size decreases from 67 to 13 nm, while the strain increases from 0.09% to 0.41%. Grain morphologies at different formation stages were observed by SEM. Saturation magnetization and coercive fields derived from the hysteresis curves are discussed as a function of milling time.     

Influence of manganese substitution and annealing temperature on the formation,microstructure and magnetic properties of Mn–Zn ferrites

The effects of annealing temperature and manganese substitution on the formation, microstructure and magnetic properties of Mn_xZn_1−xFe₂O₄ (with x varying from 0.3 to 0.9) through a solid-state method have been investigated. The correlation of the microstructure and the grain size with the magnetic properties of Mn–Zn ferrite powders was also reported. X-ray diffraction (XRD), a scanning electron microscope (SEM) and a vibrating sample magnetometer (VSM) were utilized in order to study the effect of variation of manganese substitution and its impact on crystal structure, crystalline size, microstructure and magnetic properties of the ferrite powders formed. The XRD analysis showed that pure single phases of Mn–Zn ferrites were obtained by increasing the annealing temperature to 1200–1300 °C. Increasing the annealing temperature to ?1300 °C led to abnormal grain growth with inter-granular pores and this led to a decrease in the saturation magnetization. Moreover, an increase in the Mn²⁺ ion substitution up to x=0.8 increased the lattice parameter of the formed powders due to the high ionic radii of the Mn²⁺ ion. Mn–Zn ferrites phases were formed and the positions of peaks were shifted by substituting manganese. The average crystalline size was increased by increasing the annealing temperature and decreased by increasing the substitution by manganese up to 0.8. The average crystalline size was in the range 95–137.3 nm. The saturation magnetization of the Mn–Zn-substituted ferrite powders increased continuously with an increase in the Mn concentration up to 0.8 at annealing temperatures of 1200–1300 °C. Further increase of Mn substitution up to 0.9 led to a decrease of saturation magnetization. The saturation magnetization increased from 17.3 emu/g for the Mn_0.3Zn_0.7Fe₂O₄ phase particles produced to 59.08 emu/g for Mn_0.8Mn_0.2Fe₂O₄ particles.     

Preparation and medical application of magnetic beads conjugated with bioactive molecules

Ferrite nanobeads were synthesized from an aqueous solution utilizing Fe²⁺ to Fe³⁺ oxidation for use as magnetic carriers in bioscreening, bio-molecular recognition and anti-cancer diagnosis and therapy. The beads had a crystal structure that was intermediate between Fe₃O₄ and γ-Fe₂O₃. Functional biomolecules were strongly conjugated onto the surfaces of the ferrite beads via COOH and SH groups. The addition of ferrite seed crystals (3-8 nm in size) together with a disaccharide enabled the synthesis of monodisperse, spherical ferrite beads with average diameters (d¯) between 50 and 150 nm and relative deviation Δd/d¯=9-16%. Hollow ferrite nano-spheres (d¯=150-450 nm, Δd/d¯≈10%) were prepared using silica spheres as templates, which were dissolved in NaOH solution. Ferrite beads 40 nm in size were encapsulated in polymer spheres of styrene and polymerized glycidyl methacrylate (poly-GMA), 184±9 nm in diameter. They were used for high throughput bioscreening system for affinity purification of target proteins which make specific bindings to anti-cancer drugs, porphyrins, environment hormones, etc.     

Magnetic properties of ZnFe2O4 nanoparticles produced by a low-temperature solid-state reaction method

ZnFe₂O₄ nanoparticles with average grain size ranging from 40 to 60 nm behaving superparamagnetic at room temperature have been produced using a low-temperature solid-state reaction (LTSSR) method without ball-milling process. Abnormal magnetic properties such as S-shape hysteresis loops and non-zero magnetic moments were observed. ZnFe₂O₄ nanoparticles were also synthesized using a NaOH coprecipitation method and a PVA sol-gel method to study the relationship between the preparation processes and the magnetic properties. Spin-glass behavior was observed in the low temperature solid-state reaction produced Zn ferrite in the zero-field cooled (ZFC) measurement. Our work proves that the various preparation methods will to some extent determine the properties of magnetic nanoparticles.     

Effect of nanoparticles on the magnetic properties of Mn–Zn soft ferrite

In this paper, the effect of nanostructures on the magnetic properties like the specific saturation magnetization (σ_S) and the coercivity (H_C) for Mn_0.4Zn_0.6Fe₂O₄ ferrite prepared by the co-precipitation method has been presented. We have shown by means of X-ray diffraction that the resulting ferrite is made up of nanoparticles, and that the average size of these nanoparticles calculated with the Scherrer formula depends upon the sintering temperature. When the sintering temperature is increased from 500 to 900 °C, the average nanoparticle diameter varies from 19.3 to 36.4 nm. The nanoparticle phase is further confirmed by scanning electron microscopy (SEM). Both results are found to be in good agreement. The magnetic properties are explained on the basis of the single-domain and multi-domain theory.     

Defects induced ferromagnetism in Mn doped ZnO

Single phase Mn doped (2 at%) ZnO samples have been synthesized by the solid-state reaction technique. Before the final sintering at 500 °C, the mixed powders have been milled for different milling periods (6, 24, 48 and 96 h). The grain sizes of the samples are very close to each other (～32±4 nm). However, the defective state of the samples is different from each other as manifested from the variation of magnetic properties and electrical resistivity with milling time. All the samples have been found to be ferromagnetic with clear hysteresis loops at room temperature. The maximum value for saturation magnetization (0.11 μ_B/Mn atom) was achieved for 96 h milled sample. Electrical resistivity has been found to increase with increase in milling time. The most resistive sample bears the largest saturation magnetization. Variation of average positron lifetime with milling time bears a close similarity with that of the saturation magnetization. This indicates the key role played by open volume vacancy defects, presumably zinc vacancies near grain surfaces, in inducing ferromagnetic order in Mn doped ZnO. To attain optimum defect configuration favorable for ferromagnetism in this kind of samples proper choice of milling period and annealing conditions is required.     

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.     

Magnetic properties of hexagonal ferrite dot arrays

Patterned magnetic media have been considered as one of the promising candidates for future ultra-high-density magnetic recording. In this paper, a new kind of patterned medium based on hexagonal ferrite have been studied. We have successfully fabricated strontium ferrite dot arrays by electron beam lithography. Their magnetic properties are evaluated by magnetic force microscopy (MFM) and superconducting quantum interference device (SQUID). The results show the dot arrays have perpendicular anisotropy. Dots with the lateral size larger than 500 nm show multidomain magnetization configuration in the initial magnetization state. However, with dot size decreased to 500 nm, all the dots have single-domain configuration both in the initial magnetization state and remanent magnetization state.     

Magnetic nanocomposite thin films of BaFe12O19 and TiO2 prepared by sol-gel method

The composite films with different weight ratio of barium ferrite to titanium dioxide are successfully prepared using sol-gel method for the first time. The morphology, crystal structure and magnetic properties of composite films are investigated with atomic force microscopy, X-ray diffraction and vibrating sample magnetometry. The results show that the composite films are uniform with no microcracks. The grain diameters are less than 100 nm. With the increase of barium ferrite, the grain diameter decreases. The composite films are composed of M-type hexagonal barium ferrite and rutile titanium dioxide. The composite films possess the excellent magnetic properties. The specific saturation magnetization and coercivity reach 18.3 emu/g and 3350 Oe, respectively. The application of composite films in magnetic recording and electromagnetic absorption fields is promising.     

Effect of precursor milling on magnetic and structural properties of BaFe12O19 M-ferrite

BaFe₁₂O₁₉ fine particles were synthesized after milling a precursor obtained as an intermediate in the sol–gel method. The samples were analyzed by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometry. The milling process favors the formation of the BaM phase and therefore, provides a better specific magnetization and smaller grain size compared to the same preparation route but without the milling step. We report the magnetic and structural properties of the ferrite samples obtained from milled and non-milled precursors.     

Novel combustion route of synthesis and characterization of nanocrystalline mixed ferrites of Ni-Zn

A novel combustion method of synthesis has been employed in this study for the preparation of nanoparticles of Ni-Zn ferrites. The preparation method is simple yet effective and its novelty lies in the direct mixing of reactants and the fuel. The structural and morphological studies on the nanoparticles of Ni-Zn ferrites have been carried out using X-ray diffractometer (XRD) and scanning electron microscope (SEM). The values of grain size of the ferrites obtained using the Scherrer's formula are in the range between 10 and 20 nm. The mean value of X-ray density of the Ni-Zn ferrites is around 5343 Kg/m³, which is more than the one experimentally observed for their bulk counterparts. The distribution of cations has been proposed theoretically for each concentration of Ni-Zn ferrite with reference to their respective experimental lattice constant values. Room-temperature magnetic measurements are carried out using vibrating sample magnetometer (VSM) with a view to understand the impact of the nano-regime on the magnetic parameters. The observed values of magnetization are in the range from 4 to 26 emu/g which is lower than that of bulk particles of Ni-Zn ferrite.     

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.