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.     

Induced magnetic anisotropy in Co-doped Finemet-type nanocrystalline materials

Transverse magnetic anisotropy has been induced in the Fe_14.7Co_58.8Cu₁Nb₃Si_13.5B₉ and Fe_13.8Co₆₅Cu_0.6Nb_2.6Si₉B₉ amorphous ribbons by annealing under an external magnetic field. This anisotropy plays a predominant role, compared to magneto-crystalline and magneto-elastic anisotropies, in forming the magnetic properties and shaping the hysteresis loop. The effect of temperature and time of annealing on the induced magnetic anisotropy and magnetic properties (magnetic permeability, coercivity and power losses) in both alloys was investigated. Under this work, measurements of frequency dependence of the real and imaginary parts of magnetic permeability were made within a frequency range up to 110 MHz. It was found that as a result of magnetic field annealing the Snoek limit increases in both alloys compared to the Co-free Finemet.     

Microstructure and magnetic properties of bulk amorphous and nanocrystalline Fe61Co10Zr2.5Hf2.5Nb2W2B20 alloy

The microstructure and magnetic properties, i.e. the initial magnetic susceptibility, its disaccommodation, core losses and approach to ferromagnetic saturation of the bulk amorphous and partially crystallized Fe₆₁Co₁₀Zr_2.5Hf_2.5Nb₂W₂B₂₀ alloy are studied. From X-ray, Mössbauer spectroscopy and electron microscopy studies we have stated that all samples in the as-quenched state are fully amorphous. However, after annealing the samples at 850 K for 30 min the crystalline α-FeCo grains embedded in the amorphous matrix are found. Moreover, from Mössbauer spectra analysis we have stated that the crystalline phase in those samples exhibits the long-range order. The alloy in the as-quenched state shows good thermal stability of the initial magnetic susceptibility. Furthermore, the intensity of the magnetic susceptibility disaccommodation in the rod is lower than in the ribbon. It is due to low quenching rate during the rod preparation which involves the reduction of free volumes. From the analysis of the isochronal disaccommodation curves, assuming the Gaussian distribution of relaxation times, we have found that activation energies of the elementary processes responsible for this phenomenon range from 1.2 to 1.4 eV. After the annealing of the samples the initial susceptibility slightly enhances and disaccommodation drastically decreases. From high-field magnetization studies we have learned that the size of structural defects depends on the quenching rate (the shape of the samples) and changes after annealing.     

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.     

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.     

A study of the stability of pyrolytic carbon-coated Fe/SiO2 composites in HNO3 and the effect of pyrolysis temperatures on their magnetic properties

Fe/SiO₂ composites prepared by a sol-gel combined hydrogen reduction method were coated with carbon by the pyrolysis of acetylene. Scanning electron microscopy (SEM) showed that the as-prepared sample consists of only carbon-coated Fe/SiO₂ particles without the presence of one-dimensional carbon or any other unwanted carbon formation. The stability of the Fe/SiO₂ composites under a HNO₃ solution at room temperature was greatly enhanced after they were coated with carbon. The effect of pyrolysis temperatures was also studied.     

The influence of composition and field annealing on magnetic properties of FeCo-based amorphous and nanocrystalline alloys

We report the influence of composition and very high transverse field annealing on the magnetic properties and structure of four FeCo-based amorphous and nanocrystalline alloys. The compositions (Fe₅₀Co₅₀)₈₉Zr₇B₄ and (Fe₆₅Co₃₅)₈₉Zr₇B₄ were investigated changing the Fe:Co ratio from 50:50 to 65:35. (Fe₅₀Co₅₀)₈₅Zr₂Nb₄B_8.5 was chosen to investigate Nb substitution for Zr in an FeCo-based alloy. This substitution is shown to increase the magnetostrictive constant, _λS${\lambda }_{\mathrm{S}}$, of the nanocrystalline alloy from 36×10⁻⁶ to 54×10⁻⁶. The composition (Fe₆₅Co₃₅)₈₄Cr₅Zr₇B₄ was studied to investigate the influence of Cr on intergranular coupling across the amorphous matrix. Samples of each composition were annealed in the amorphous state at 300 °C and in the nanocrystalline state at 600 °C. Field annealing was performed in 17 T transverse field in an inert atmosphere. Frequency-dependent magnetic properties were measured with an automatic recording hysteresisgraph. Static magnetic properties were measured with a vibrating sample magnetometer. The mass-specific power loss of the alloys decreased with field annealing in both the nanocrystalline and amorphous states for some frequency and induction combinations. Furthermore, the hysteresis loops are sheared after field annealing, indicating a transverse magnetic anisotropy. The nanocrystalline (Fe₅₀Co₅₀)₈₅Zr₂Nb₄B_8.5 composition has a lower relative permeability than the other compositions.     

A study on microstructure,magnetic properties and kinetics of the nanocrystallization of Fe40Ni38B18Mo4 metglass

This study has investigated the microstructure and magnetic properties of Fe₄₀Ni₃₈B₁₈Mo₄ at various degrees of crystallization from the amorphous state. TEM and XRD studies confirmed that phases forming after crystallization at temperatures around 414 and 522 °C were cubic (Fe, Ni, Mo)₂₃B₆ phase and FCC (Fe, Ni) solid solution. The growth behavior and morphology of the nanocrystalline phases have been studied as a function of time and temperature. Nanoparticles were lying in the size range of 10–20 nm and they were stable below 522 °C. Kissinger approach, Ozawa method and Yi Qun Gao method were employed to determine and compare the kinetic parameters of the crystallization processes. A growth mechanism of crystallizing phases was proposed on the basis of these results. Magnetic properties mainly coercivity and saturation magnetization of as-received and heat-treated samples were evaluated.     

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.     

Electromagnetic wave absorption properties of Fe3C/carbon nanocomposites prepared by a CVD method

Dendrite-shaped iron nanowires with 50-200 nm in diameter and 10-20 μm in length were prepared by the CVD method from Fe(CO)₅ as a starting source. Ethanol was cracked on the surface of the resultant iron nanowires to form the Fe₃C/carbon nanocomposites, in which nanosized carbon beads covered the surface of Fe₃C. Resin compact of the resultant Fe₃C/carbon nanocomposites had excellent electromagnetic wave absorption ability in the range of 0.9-9.0 GHz, and such available absorption range more enhanced compared to that observed on the resin compact prepared from the original iron nanowires by the hybridization of magnetic (Fe₃C) and dielectric (carbon) materials.     

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.     

Growth of single-crystal magnetite nanowires from Fe3O4 nanoparticles in a surfactant-free hydrothermal process

Single-crystal magnetite nanowires with average diameter of ca. 20 nm and length of up to several micrometers were prepared by a simple alkaline surfactant-free hydrothermal process. The crystallinity, purity, morphology, and structural features of the as-prepared magnetite nanowires were investigated by powder X-ray diffraction, transmission electron microscopy (TEM) and selected area electron diffraction. The composition and length of nanowires depends on the pH, with higher pH favoring longer nanowires composed entirely of Fe₃O₄. A mechanism for nanowire growth is proposed.     

Modelling magnetic polarisation J50 by different methods

Two different methods for modelling the angular behaviour of magnetic polarisation at 5000 A/m (J₅₀) of electrical steels were evaluated and compared. Both methods are based upon crystallographic texture data. The texture of non-oriented electrical steels with silicon content ranging from 0.11 to 3%Si was determined by X-ray diffraction. In the first method, J₅₀ was correlated to the calculated value of the average anisotropy energy in each direction, using texture data. In the second method, the first three coefficients of the spherical harmonic series of the ODF and two experimental points were used to estimate the angular variation of J₅₀. The first method allows the estimation of J₅₀ for samples with different textures and Si contents using only the texture data, with no need of magnetic measurement, and this is advantageous, because texture data can be acquired with less than 2 g of material. The second method may give better adjust in some situations but besides the texture data, it requests magnetic measurements in at least two directions, for example, rolling and transverse directions.     

Curie temperatures and crystallization behavior of amorphous Fe81−xNixZr7B12 (x=10, 20, 30, 40, 50, 60) alloys

Curie temperature, crystal structure and crystallization behavior of amorphous alloys with the stoichiometry Fe_81−xNi_xZr₇B₁₂ (x=10–60) have been studied by X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and AC-magnetization (TMAG) measurements as functions of temperature. The thermal stability of long-range magnetic order, T_C vs. Ni content in as-quenched amorphous alloys exhibits maximum at 352 °C for x=40. The primary crystallization has been detected during annealing at the first crystallization stage of all ribbons investigated.     

Structural and magnetic properties of SrFe12O19 hexaferrite synthesized by a modified chemical co-precipitation method

M-type strontium hexaferrite (SrFe₁₂O₁₉) particles had been prepared by a modified chemical co-precipitation route. Structural and magnetic properties were systematically investigated. Rietveld refinement of X-ray powder diffraction results showed that the sample was single-phase with the space group of P6₃/mmc and cell parameter values of a=5.8751 Å and c=23.0395 Å. The results of field-emission scanning electronic microscopy showed that the grains were regular hexagonal platelets with sizes from 2 to 4 μm. The composition determined by energy dispersive spectroscopy is the stoichiometry of SrFe₁₂O₁₉. The ferrimagnetic to paramagnetic transition was sharp with Curie temperature T_C=737 K, which further confirmed that the samples were single phase. However, it was found that the coercivity, saturation magnetization and the squareness ratio of the synthesized SrFe₁₂O₁₉ samples were lower than the theoretical values, which could be explained by the multi-domain structure and the increase of the demagnetizing factor.     

Crystallization of Fe75Zr25 metallic glass: a two‐step process involving metastable bcc‐Fe and polymorphic transformation

The crystallization process of mechanically alloyed Fe₇₅Zr₂₅ metallic glasses is investigated by means of both thermo‐magnetization and in situ neutron powder thermo‐diffraction experiments in the temperature range 300–1073 K. It was found that the crystallization takes place in a two‐step process, involving firstly the appearance of metastable Fe and Fe₂Zr crystalline phases between 880 K and 980 K, and a subsequent polymorphic transformation into Fe₃Zr above 980 K. These findings explain the anomalous magnetization vs. temperature behaviour on heating–cooling cycles.

     

Effect of SiO2 nanopowders on magnetic properties and corrosion resistance of sintered Nd-Fe-B magnets

To improve the magnetic properties and corrosion resistance of magnet, SiO₂ nanopowders were added into Nd_28.25Dy_2.75Fe_balAl_0.15Ga_0.1Nb_0.1B_0.98-sintered magnets as grain boundary modifiers. It was found that the intrinsic coercivity (H_cj), remanence (B_r) and corrosion resistance were all improved with addition of certain amount of SiO₂ nanopowders. The optimum addition amount of SiO₂ nanopowders was found to be 0.01 wt%. Thermodynamic calculation in combination of energy dispersive X-ray spectroscopy (EDX) analyses indicated that SiO₂ nanopowders reacted with Nd of Nd-rich phase. As a result, the intergranular phase was modified, and the grain growth of main phase was restrained. It led to the optimization of microstructure.     

Annealing effect on soft magnetic properties and magnetoimpedance of Finemet Fe73.5Si13.5B9Nb3Au1 alloy

Effect of annealing on the soft magnetic properties of Fe_73.5Si_13.5B₉Nb₃Au₁ amorphous ribbon has been investigated by means of structure examination, magnetoimpedance ratio (MIR) and incremental permeability ratio (PR) spectra measured in the frequency range of 1–10 MHz at a fixed current of 10 mA X-ray diffraction analysis showed that the as-cast sample was amorphous and it became nanocrystalline under a proper heat treatment. When annealing amorphous alloy at 530 °C for 30, 60, 90 min, soft magnetic properties have been improved drastically. Among the samples investigated, the sample annealed at 530 °C for 90 min showed the softest magnetic behavior. The MIR and PR curves revealed the desirable changes in anisotropy field depending upon annealing.     

Structural,microstructural and magnetic properties of nanocomposite isotropic Sm(CobalFe0.1MyZr0.04B0.04)7.5 ribbons with M=Ni,Cu and y=0.09 and 0.12

In boron-substituted melt-spun Sm(Co,Fe,Cu,Zr)_7.5-type alloys a nanocomposite microstructure and high coercivities in both as-spun and short-time annealed ribbons can be obtained. In the present study three different compositions, namely Sm(Co_0.73Fe_0.1Cu_0.09Zr_0.04B_0.04)_7.5, Sm(Co_0.70Fe_0.1Cu_0.12Zr_0.04B_0.04)_7.5 and Sm(Co_0.70Fe_0.1Ni_0.12Zr_0.04B_0.04)_7.5 have been examined in order to investigate the influence of composition on the magnetic properties and the microstructure. Melt-spun ribbons have been obtained and annealing has been followed under argon atmosphere for 30–75 min at 600–870 °C. For the as-spun ribbons the TbCu₇-type of structure and fcc-Co as a secondary phase have been identified in the X-ray diffraction patterns. For the annealed ribbons above 700 °C the 1:7 phase transforms into 2:17 and 1:5 phases. The TEM studies have shown a homogeneous nanocrystalline microstructure with average grain size of 30–80 nm. Coercivity values of 15–27 kOe have been obtained from hysteresis loops traced in non-saturating fields. The coercivity decreases with temperature, but it is sufficiently large to maintain values higher than 5 kOe at 380 °C.