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.     

Structure and magnetic properties of nanocrystalline Fe75Si25 powders prepared by mechanical alloying

Nanocrystalline Fe₇₅Si₂₅ powders were prepared by mechanical alloying in a planetary ball mill. The evolution of the microstructure and magnetic properties during the milling process were studied by X-ray diffraction, scanning electron microscope and vibrating sample magnetometer measurements. The evolution of non-equilibrium solid solution Fe (Si) during milling was accompanied by refinement of crystallite size down to 10 nm and the introduction of high density of dislocations of the order of 10¹⁷ m⁻². During the milling process, Fe sites get substituted by Si. This structural change and the resulting disorder are reflected in the lattice parameters and average magnetic moment of the powders milled for various time periods. A progressive increase of coercivity was also observed with increasing milling time. The increase of coercivity could be attributed to the introduction of dislocations and reduction of powder particle size as a function of milling time.     

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).     

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.     

Preparation of nanocrystalline Fe–Ni powders by mechanical alloying used in soft magnetic composites

This paper focuses on the preparation of nanocrystalline Fe–Ni powders by mechanical alloying method, which can be used in soft magnetic composites. Fe–10 wt% Ni and Fe–20  wt % Ni alloys were prepared using a high-energy ball mill. The magnetic properties of samples were measured by a B–H curve analyzer and microstructures of the samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The bcc Fe(Ni) phase formation was identified by XRD and completed after 45 h of milling. It was found that higher milling time resulted in, larger lattice parameter, higher microstrains and smaller crystallite sizes. Also, results showed that with increasing the milling time, coercivity increased and saturation intrinsic flux density firstly increased noticeably and then decreased in higher milling times (>70 h).     

Effects of powder flowability on the alignment degree and magnetic properties for NdFeB sintermagnets

The magnetic powders for sintered NdFeB magnets have been prepared by using the strip casting (SC), hydrogen decrepitation (HD) and jet milling (JM) techniques. The effects of powder flowability and addition of a lubricant on the alignment degree and the hard magnetic properties of sintered magnets have been studied. The results show that the main factor affecting powder flowability is the aggregation of magnetic particles for powders in a loose state, but it is the friction between the powder particles for powders that are in a compact state. The addition of a lubricant with suitable dose can slightly prevent the congregating of powders, obviously decrease the friction between the powder particles, improve the powder flowability, and increase the alignment degree, remanence and energy product density of sintered magnets. Mixing a suitable dose of lubricant and adopting rubber isostatic pressing (RIP) with a pulse magnetic field, we have succeeded in producing the sintered NdFeB magnet with high hard magnetic properties of B_r=14.57 KG, _jH_c=14.43 KOe, (BH)_max=51.3 MGOe.     

Simultaneous variations of microstructure and magnetic properties of Ni58Fe12Zr20B10 nanostructure/amorphous alloy prepared by mechanical alloying

This study aims to evaluate magnetic and micro-structural properties of amorphous/nanocrystalline mechanically alloyed Ni₅₈Fe₁₂Zr₂₀B₁₀ powders with ball-milling time up to 190 h. Structural, micro-structural and thermal evaluations of the milled powders were carried out by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM) and differential scanning calorimetry (DSC) methods. Magnetic properties were also measured by a vibrating sample magnetometer (VSM) instrument. Results showed that the amorphous phase reached maximum value of 95% and the crystallite size was about 3 nm at the end of the milling. Magnetization saturation (M_s) decreased slightly and coercivity (H_c) reached to the highest value at 72 h of the milling time. At the 190 h of milling, the coercivity and saturation magnetization reached 18 Oe and 20 emu/g, respectively. While, after an appropriate amount of heat treatment, these two variables became approximately 2 Oe and 32 emu/g.     

Characterization of nanocrystalline FeSiCr powders prepared by ball milling

FeSi₁₀Cr₁₀ powder was mechanically alloyed by high energy planetary ball milling, starting from elemental powders. The microstructural and magnetic properties of the milled powders were characterized by scanning electron microscopy, X-ray diffraction, ⁵⁷Fe Mössbauer spectrometry and a vibratory sample magnetometer.After 3 h of milling, the formation of two bcc solid solutions α-Fe₁ (Si, Cr) and α-Fe₂ (Si, Cr) is observed. Their grain sizes decrease with increase in milling time attaining, at 15 h of milling, 23 and 11 nm, respectively. Mössbauer spectra of the milled powder show the presence of two components. One is a ferromagnetic type with a broad sextuplet. Its distribution of hyperfine field is characterized by high and low hyperfine field’s peaks and a mean value of 26.5 T. The other is a single paramagnetic peak. Its low concentration increases to ∼4% at 15 h of milling. These results can be explained by different atomic environments affected by Si or/and Cr elements, as well as the increased disordered grain boundaries.Magnetic measurements of the milled FeSi₁₀Cr₁₀ alloy powder exhibit a soft ferromagnetic character with a decrease of both magnetization at saturation (Ms) and coercive force (Hc) with milling time attaining values of Ms=151 emu/g and Hc=2500 A/m at 30 h of milling time.     

Study of nanocrystalline and amorphous powders prepared by mechanical alloying

The process of mechanical alloying consists of intimate mixing and mechanical working of elemental powders in a high-energy ball mill. It has been well established that this process is able to produce nanocrystalline and amorphous material. In this study, the structural effects of mechanical alloying of pure Fe, Fe₅₀W₅₀ and Fe₅₀Mo₅₀ powders were investigated by X-ray diffraction and Mössbauer spectroscopy. For all cases, nanocrystalline and/or amorphous fractions were found after milling. The resulting particle size was determined by X-ray diffraction. Pure Fe does not amorphize even after prolonged milling times. For the nanocrystalline powder, significant changes in the linewidth and the hyperfine field are found. Powder mixtures of Fe₅₀Mo₅₀ and Fe₅₀W₅₀ are completely amorphous after milling times of 10 h, as seen by Mössbauer spectroscopy, but nanocrystalline fractions of the non-iron part are still found in X-ray diffraction. Also in the amorphous state, further changes in the hyperfine parameters are found with increasing milling time.     

Evolution of structure, microstructure and hyperfine properties of nanocrystalline Fe50Co50 powders prepared by mechanical alloying

Nanostructured Fe₅₀Co₅₀ powders were prepared by mechanical alloying of Fe and Co elements in a vario-planetary high-energy ball mill. The structural properties, morphology changes and local iron environment variations were investigated as a function of milling time (in the 0-200 h range) by means of X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray analysis and ⁵⁷Fe Mössbauer spectroscopy. The complete formation of bcc Fe₅₀Co₅₀ solid solution is observed after 100 h milling. As the milling time increases from 0 to 200 h, the lattice parameter decreases from 0.28655 nm for pure Fe to 0.28523 nm, the grain size decreases from 150 to 14 nm, while the meal level of strain increases from 0.0069% to 1.36%. The powder particle morphology at different stages of formation was observed by SEM. The parameters derived from the Mössbauer spectra confirm the beginning of the formation of Fe₅₀Co₅₀ phase at 43 h of milling. After 200 h of milling the average hyperfine magnetic field of 35 T suggests that a disordered bcc Fe-Co solid solution is formed.     

A structural,magnetic and microwave study on mechanically milled Fe-based alloy powders

Fe₉₀M₁₀ powders with M=Fe, Co, Ni, Si, Al, Gd, Dy and Nd were prepared by mechanical milling. Their structure and magnetic properties were investigated. Microwave measurements were performed on the mechanically milled Fe₉₀M₁₀ powders. The results were compared with those of carbonyl Fe powders and coarse Fe powder. It has been shown that fine nanocrystalline Fe-based alloy powders prepared by mechanical milling are promising for microwave applications.     

Highly anisotropic resin-bonded magnets processed with surfactant-coated SmCo5 nanocrystalline powders

Highly anisotropic SmCo₅ nanocrystalline powders with grain size in the range 5-20 nm were processed through surfactant and magnetic field-assisted milling. The SmCo₅ nanocrystalline powders so obtained by this method possess unusual characteristics such as reduction in particle size, platelet-structure and high remanence values. A possible mechanism for achieving remanence enhancement with the surfactant-coated SmCo₅ powders has been discussed. Besides, the resin-bonded magnets processed with the surfactant-coated SmCo₅ powders showed relatively higher density, induction remanence and energy product with strong anisotropic behavior than those of the magnets processed with the conventionally milled SmCo₅ powders. Maximum values of H_ci (16 kOe), B_r (4.66 kG) and (BH)_max (5.5 MG Oe) were achieved for the resin-bonded magnets processed with the surfactant-coated powders.     

Influence of acid catalysts on the structural and magnetic properties of nanocrystalline barium ferrite prepared by sol–gel method

BaFe₁₂O₁₉ powders with nanocrystalline size were prepared by sol–gel techniques. Nitric, hydrochloric, acetic and stearic acid were used to improve the magnetic properties. Amorphous gels were formed with Fe/Ba molar ratio of 10.5. Then powders were obtained by subsequent heat treatment at 800–1000 °C for 1 h. Barium ferrite powder was also synthesized by solid state reaction at 1210 °C. X-ray diffraction, scanning electron microscopy and transmission electron microscopy (TEM) experiments were conducted to evaluate structural properties of the samples. The value of the effective magnetic susceptibility was measured. The results show that the magnetoplumbite structure was formed in all of the powders. The TEM observation showed that the minimum particle size (20 nm) was produced with the stearic acid catalyst. The highest value of the effective magnetic susceptibility was achieved also using stearic acid.     

The structural and magnetic properties of one-step mechanochemical route synthesized La0.8Pb0.2MnO3 manganites

Mechanochemical route has been used to produce La_0.8Pb_0.2MnO₃ (LPMO) nanocrystalline samples from oxide precursors. The samples were characterized using X-ray diffraction, scanning electron microscope and AC susceptibility measurements. The results showed that it is possible to produce LPMO perovskite powders after 10 h of ball milling. The crystallite size and microstrain were estimated using Williamson-Hall equation. The results showed that the crystallite size and microstrain increase initially and then decrease by the increase of milling time. By decreasing particle size the dislocation density (strain) increases and reaches to a saturation point at a particular particle size, further particle size reduction takes place through gliding motion along grain boundaries, which leads to a reduction of the strain. The dynamic properties of 15 h ball-milled sample were investigated by AC susceptibility using the Neel-Brown and Vogel-Fulcher law for superparamagnetism. The frequency dependence of blocking temperature is well described by the Vogel-Fulcher law, and fitting the experimental data with Neel-Brown law gives unphysical value for relaxation time.     

Anisotropy models in precise crystallite size determination of mechanically alloyed powders

Nanocrystalline AA 4032 alloy powder was synthesized by high-energy ball milling from elemental powders for 30 h duration. XRD and TEM results reveal that the powder is cubic and nanocrystalline in nature. X-ray peak broadening analysis was used to evaluate the lattice strain and the crystallite size using the Williamson-Hall analysis with three different models viz., uniform deformation, uniform deformation stress and uniform deformation energy density. The root mean square (RMS) strain was calculated from the interplanar spacing and the strain estimated from the three models. The three models yield different strain values due to the anisotropic nature of the material. The energy density model is proposed to be the best fit model among the three as severe lattice strain is associated with ball milled powders.     

Enhancement of electromagnetic and microwave absorbing properties of gas atomized Fe-50 wt%Ni alloy by shape modification

In order to increase the electromagnetic parameters and improve the microwave absorbing properties in the range of 1–4 GHz, gas atomized Fe-50 wt%Ni alloys with spherical form were processed in a planetary mill. The morphology, phase composition and saturation magnetization of the FeNi alloy particles were investigated by means of scanning electron microscopy, X-ray diffraction and vibrating sample magnetometer. The complex permittivity, complex permeability and reflection loss of the microwave absorbing material made from Ethylene–Propylene–Diene Monomer rubber, and the Fe-50 wt%Ni alloys were also studied using vector network analyzer and transmission line theory. The results show that the shape of the atomized Fe-50 wt%Ni powders can be modified by mechanical milling. The flaky Fe-50 wt% Ni particles were prepared, and the aspect ratio increases with increasing the milling time from 10 to 30 h. Mechanical milling does not change the phase compositions of the FeNi alloys but decreases the peak intensity and broadens the peak width. The saturation magnetization decreases and the coercivity increases as the milling time increases. The electromagnetic parameters and microwave absorbing properties are enhanced with the increase of the aspect ratio. The rubber absorbers filled with flaky Fe-50 wt%Ni powders milled for 30 h exhibit the low reflection loss in the 1–4 GHz frequency range.     

Structural and magnetic properties of Co50Ni50 powder mixtures

In the present work, morphological, structural, thermal and magnetic properties of nanocrystalline Co₅₀Ni₅₀ alloy prepared by high energy planetary ball milling have been studied by means of scanning electron microscopy, X-ray diffraction, and differential scanning calorimetry. The coercivity and the saturation magnetization of alloyed powders were measured at room temperature by a vibration sample magnetization. Morphological observations indicated a narrow distribution in the particle and homogeneous shape form with mean average particle size around 130 μm². The results show that an allotropic Co transformation hcp→fcc occurs within the three first hours of milling and contrary to what expected, the Rietveld refinement method reveals the formation of two fcc solid solutions (SS): fcc Co(Ni) and Ni(Co) beside a small amount of the undissolved Co hcp. Thermal measurement, as a function of milling time was carried out to confirm the existence of the hcp phase and to estimate its amount. Magnetic measurement indicated that the 48 h milled powders with a steady state particles size have the highest saturation (105.3 emu/g) and the lowest coercivity (34.5 Oe).     

Crystallization of mechanically alloyed amorphous W-Mg alloy under high pressure

Pure metal powder mixtures of W and Mg at the desired composition were milled in conventional high-energy ball mill, and amorphous alloy W₅₀Mg₅₀ was obtained after milling for 20 h. The structure evolution of elemental powder mixtures was studied following milling and subsequent high pressure and high temperature treatment. The amorphous alloy transform into a nanocrystalline material below 1050 °C at 4.0 GPa. On increasing the temperature, it transforms into a mixture of several new crystal phases under high-pressure condition. It also found that both mechanical alloying and high pressure treatment are the two necessary processes to form the nanocrystalline and the new phases.     

The effect of multi-step milling and annealing treatments on microstructure and magnetic properties of nanostructured Fe-Si powders

Nanostructured Fe_1−xSi_x (x=0.05, 0.1, 0.15 and 0.2) powders are prepared by different multi-step milling and annealing treatments. The microstructure and magnetic properties are investigated for all alloys. The minimum crystallite size of as-annealed powders (∼40 nm) is found to be larger than in as-milled ones (∼15 nm). It is found that microstrains of 2- and 4-step processes are close to those of the as-received powders. The lattice parameter decreased ∼0.5% and 0.9% for the powders that experienced milling and annealing at the last step, respectively. The Fe₈₀Si₂₀ powders prepared by 1- and 4-step treatments show the maximum (40-125 Oe) and minimum (20-26 Oe) coercivity, respectively. With increase in milling time, mass magnetization increased for all processes. This can be ascribed to diminution in magneto-crystalline anisotropy due to grain refinement. The maximum mass magnetization (160-199 Am²/kg) is achieved for the 4-step process.     

Study of magnetic phases in mechanically alloyed Fe50Zn50 powder

The mechanosynthesis of Fe₅₀Zn₅₀ alloy resulted in the formation of the bcc Fe(Zn) solid solution after 20 h of milling. Structural transformations induced by mechanical alloying and heating, and magnetic properties of the powders were studied by Mössbauer spectroscopy, X-ray diffraction, Faraday balance and vibrating sample magnetometry techniques. All alloys studied exhibit strong magnetic ordering with Curie temperatures close to 900 K. Room temperature Mössbauer measurements revealed distinguished magnetic environments in the samples. The decrease of coercivity with prolonged milling time was attributed to the reduction or averaging of local magnetic anisotropies.