Optimisation of soft magnetic properties in Fe–Cu–X–Si13B9 (X=Cr,Mo, Zr) amorphous alloys

In the present paper a group of Fe–Cu–X–Si₁₃B₉ (X=Cr, Mo, Zr) amorphous alloys has been examined by applying different experimental techniques—magnetic permeability, magnetic after-effect, coercive force and electrical resistivity measurements. It has been shown that their soft magnetic properties can be optimised by 1-h thermal annealing at the temperature close to the crystallisation temperature. This leads to an increase of permeability and a decrease of coercive force, thermal instability (magnetic after-effect intensity) and electrical resistivity of the material. The optimisation effect is discussed in terms of different processes—(i) a formation of a nanocrystalline phase with the grain size much smaller than the ferromagnetic exchange length, (ii) an annealing out of microvoids formed during the fabrication process and also (iii) a decrease of the effective magnetostriction constant. The temperature of optimisation annealing treatment is always higher than the Curie temperatures of the materials and varies approximately linearly with the atomic radius of the alloying additions.     

Nanocrystallization process and ferromagnetic properties of amorphous (Fe0.99Mo0.01)78Si9B13 ribbons

The nanocrystallization process of soft ferromagnetic (Fe_0.99Mo_0.01)₇₈Si₉B₁₃ ribbons has been studied in detail. Microstructural and ferromagnetic properties are examined by transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy (MS), differential scanning calorimetry (DSC) and magnetization measurements. The Curie and crystallization temperatures are determined to be T_C=665 K and T_x=750 K, respectively. The T_x value is in well agreement with DSC measurement results. XRD patterns had shown two metastable phases (Fe₂₃B₆, Fe₃B) which were formed under in situ nanocrystallization process. These metastable phases embedded in the amorphous matrix have a significant effect on magnetic ordering. The ultimate nanocrystalline (NC) phases of α-Fe(Mo, Si) and Fe₂B at optimum annealing temperature had been observed respectively. It is notable that the magnetization of the amorphous phase decreases more rapidly with increasing temperature than those of NC ferromagnetism, which suggest the presence of the distribution of exchange interaction in the amorphous phase or high metalloid contents.     

FeCo基纳米晶合金高温交换耦合作用机理

研究了500和600℃真空退火后的纳米晶Fe_38.4Co₄₀Si₉B₉Nb_2.6Cu合金初始磁导率随温度的变化规律,发现较高温度(600℃)退火的FeCo基纳米晶合金,在非晶相居里温度以上较宽温度范围内磁导率没有明显的衰减,这是在双相纳米晶合金中观察到的一种新现象,其磁特性不同于Fe基纳米晶合金.为了探明这种现象的起源,估算了与剩余非晶相同成分的非晶合金的居里温度及纳米晶粒间发生交换耦合作用的参数 关键词： 交换耦合作用 非晶相居里温度 交换耦合穿透深度     

Detailed study of ultra-soft magnetic properties of Fe74Cu0.8Nb2.7Si15.5B7

The magnetic properties of nanocrystalline Fe₇₄Cu_0.8Nb_2.7Si_15.5B₇ alloy, which were rapidly solidified and then annealed at various temperatures between 475 and 650°C for different holding time, have been studied. Grain size, silicon content and the lattice parameter of α-Fe(Si) nanograins at the annealing temperatures were determined. Curie temperature of the amorphous phase was determined from the temperature dependence of permeability. For higher annealing temperatures and times, some Si diffused out of the α-Fe(Si) phase and formed an ordered DO₃ phase of Fe₃Si. This changed the overall magnetostriction and average anisotropy of the matrix, which deteriorated the magnetic softness of the material at higher annealing temperatures. Ultra-soft magnetic properties were achieved by averaging the random anisotropy via exchange interaction. Hysteresis loops for samples in as-cast and annealed conditions have also been studied.     

Magnetic Behavior of Nanocrystalline FeNbCrBCu Alloys at Elevated Temperatures

The magnetic behavior of nanocrystalline Fe_73.5Nb_4.5Cr₅B₁₆Cu₁ alloys is investigated in a series of specimens with different volume fractions of crystalline phase. It is shown that the Curie temperature of amorphous phase firstly decreases after structural relaxation in amorphous state and then rapidly increases during the first stages of crystallization. The strikingly different behavior of coercivity at elevated temperatures is observed for the samples with low and high volume fractions of nanocrystalline particles.     

Temperature dependence of amorphous and interface phases in the Fe80Nb7Cu1B12 nanocrystalline alloy

Temperature measurements (77–625 K) of Fe₈₀Nb₇Cu₁B₁₂ nanocrystalline alloy prepared from amorphous precursor annealed for 1 h at 470^°C and 620^°C are presented. Structural and magnetic behaviours of the crystalline phase, the amorphous residual matrix, and the interface zone between crystalline grains and the amorphous phase are studied by distributions of hyperfine magnetic fields. Magnetic regions are developing in the retained amorphous phase with rising temperature of annealing. They can be suppressed, however, at high enough measuring temperatures turning the amorphous matrix into paramagnetic state. As a consequence, the respective spectral components do not interfere so much and the role of interface zone can be studied. This revised version was published online in July 2006 with corrections to the Cover Date.     

Grain growth process of two-phase nanocrystalline soft magnetic materials

In order to clarify the origin of the high thermal stability of the microstructure in bcc-Fe/amorphous two-phase nanocrystalline soft magnetic materials, we have investigated the changes in the magnetic and microstructural properties upon isothermal annealing at 898 K for an Fe₈₉Zr₇B₃Cu₁ alloy by means of transmission electron microscopy, Mössbauer spectroscopy and DC magnetometry. The mean grain size was found to remain almost unchanged at the early stage of annealing. However, rapid grain coarsening was evident at an annealing time of 7.2 ks where the intergranular amorphous phase begins to crystallize into Fe₂₃Zr₆. The grain growth process with a kinetic exponent of 1.6 is observed for the growth process beyond this annealing time, reflecting the disappearance of the intergranular amorphous phase. Our results confirm that the thermal stability of the bcc-Fe/amorphous two-phase nanocrystalline soft magnetic alloys is governed by the residual amorphous phase.     

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.     

Observations of magnetic coupling in Fe-based nanocrystalline alloy by high-temperature giant magneto-impedance effect

The giant magneto-impedance (GMI) effect for Fe_73.5Cu₁Nb₃Si_13.5B₉ nanocrystalline ribbons is investigated in the temperature range between room temperature and 873 K. The thermal dependence of GMI effect reveals the enhancement of Curie temperature of the amorphous matrix, reflecting the exchange coupling between the α-FeSi grains as well as the compositional changes of the amorphous matrix itself. However, the dipolar interaction between grains is suggested to be responsible for the non-zero GMI effect after the magnetic phase transition of the amorphous matrix.     

Effect of nitrogen concentration on the magnetic properties of Fe-Ta-N thin films

Soft magnetic nanocrystalline thin films with a high content of Ta (10 wt %) are synthesized by the method of reactive RF magnetron sputtering with subsequent annealing. It is established that the microstructure and magnetic properties of the films depend on the nitrogen partial pressure during sputtering and on the annealing temperature. Annealing of the amorphous films leads to the formation of α-Fe nanocrystallites whose properties and interactions determine the film parameters. A decrease in the α-Fe grain size to a level below the length of ferromagnetic exchange interaction sharply increases the magnetic softness. The role of nitrogen ions in the formation of a α-Fe nanocrystallite structure and uniaxial magnetic anisotropy of Fe-Ta-N films is established. The optimum technological regimes of deposition and annealing of the Fe-Ta-N films are determined, which ensure the synthesis of Fe-Ta-N nanocrystalline thin films with a high magnetic softness (B _s=1.6 T, H _c=0.2 Oe, and μ₁(1 MHz)=3400).     

Amorphous Heusler alloys: The effect of annealing on structure and magnetic and transport properties

Alloys with the Heusler compositions Cu₂MnIn, Cu₂MnAl and Cu₂MnSn have been prepared as amorphous films for the first time. The structural disorder results in as-deposited films which are not ferromagnetic and, in fact, exhibit spin-glass properties due to the distribution of MnMn distances and co-existence of positive and negative exchange interactions. Annealing of the In and Al alloys can restore single phase ordered Heusler structures which are ferromagnets with Curie temperatures typical of bulk alloys. The calculated Mn moments remain lower than the bulk values of 4 μ_B probably due to disorder at grain boundaries. Films annealed under non-optimum conditions crystallized into several non-magnetic structures as well as the magnetic L2₁ Heusler phase. Lattice constants of all phases were determined. The temperature dependence of resistivity through the amorphous-crystalline transformation was found to confirm the results of thermal annealing on structure and magnetization.     

Thermal behavior for a nanoscale two ferromagnetic phase system based on random anisotropy model

Advances in theory that explain the magnetic behavior as function of temperature for two phase nanocrystalline soft magnetic materials are presented. The theory developed is based on the well known random anisotropy model, which includes the crystalline exchange stiffness and anisotropy energies in both amorphous and crystalline phases. The phenomenological behavior of the coercivity was obtained in the temperature range between the amorphous phase Curie temperature and the crystalline phase one.     

Progress of laser spectroscopy at the IGISOL

Magnetic interactions and microstructure in the amorphous and nanocrystalline Fe₉₀Zr₇Cu₁B₂ alloy were investigated. These studies were carried out in the temperature range from 140 up to 380 K, using a Mössbauer spectrometer and completely automated set-up for measurements of magnetic properties. It has been found that the Curie temperature and quadrupole splitting decrease after annealing the sample at 573 K for 1 h (invar effect). However, this behaviour is not observed in nanocrystalline samples. In the early stages of crystallization (the volume fraction of the crystalline phase equal to about 0.06) α-Fe grains above the Curie temperature of amorphous matrix may be treated as non-interacting particles. The particle size estimated by Mössbauer spectra and magnetization curve analysis is equal to about 4 nm.     

非晶态Fe90-xBxZr10合金的磁性、电性和晶化

本文研究了部分B元素替代Fe对非晶态FeZr基合金磁性、电性和晶化的影响,并与非晶态FeB合金作了比较。解释了样品中每个FeZr原子的平均磁矩μ_FeZr和居里温度T_c随B含量x的增加而增加的原因,讨论了在不同的温区样品中可能存在的散射机制对电阻率的贡献以及影响晶化温度的因素。 关键词：     

Anomalous magnetism of the nanocrystalline oxide TiO<Subscript>2</Subscript> surface

The magnetic properties of an oxygen-deficient nanocrystalline undoped titanium dioxide synthesized by the gas-phase, electric-explosion, and chemical method have been studied. The defect state was controlled using reduction treatments in vacuum or in a hydrogen atmosphere. It is shown that the defect state of the surface of nanocrystalline oxides (for example, the existence of vacancies in the anion sublattice and other defects) has a dominant influence on the formation of the magnetic properties of the samples under study. The main contributions to the magnetism of TiO₂ nanoparticles after the reduction treatments are the paramagnetic contribution of the matrix, the paramagnetic Curie–Weiss contribution, and the contribution of the spontaneous magnetic moment provided by the existence of regions with different spin ordering. A heterogeneous magnetic state is found to exist in the TiO₂ nanopowders; for example, at low temperatures, shifted hysteresis loops are observed as a result of a possible set of magnetic states with different spin orders. It is shown that a soft compaction or grinding of nanopowders in an agate mortar lead to substantial increase in the magnetization, sometimes, by a factor of more than two, regardless of the nanopowder synthesis method and the initial phase state of TiO₂ (anatase or rutile structures). This experimental fact proves the key role of the surface defects and the magnetic moment carriers with different spin configurations localized mainly on the nanoparticle surface. The compaction changes the magnetization only in the case when the initial magnetic state has a nonlinear “quasi-superparamagnetic” character of the magnetization curve. As a result of predominant exchange interaction between the nanoparticles with a frustrated character of spin ordering on the nanoparticles surface, the ferromagnetic contribution increases as nanoparticles contact.     

Properties of ferromagnetic resonance in Fe<Subscript>73.5</Subscript>CuNb<Subscript>3</Subscript>Si<Subscript>13.5</Subscript>B<Subscript>9</Subscript> nanocrystalline alloys

The structural properties and parameters of ferromagnetic resonance have been studied for Fe_73.5CuNb₃Si_13.5B₉ nanocrystalline alloys produced from the initial amorphous state via annealing under different conditions. The dependence of the linewidth of the ferromagnetic resonance on the grain size ΔH ∼ D ⁶ has been found. The result is discussed within the framework of the random magnetic anisotropy model.     

Influence of composition on hyperfine interactions in FeMoCuB nanocrystalline alloy

Influence of varying Fe/B ratio upon hyperfine interactions is investigated in the Fe_91?x Mo₈Cu₁B_x rapidly quenched alloys. They are studied both in the as-quenched (amorphous) state as well as after one-hour annealing at different temperatures ranging from 330 °C up to 650 °C. Such a heat treatment causes significant structural changes featuring a formation of nanocrystalline bcc-Fe grains during the first crystallization step. At higher annealing temperatures, a grain growth of bcc-Fe and occurrence of additional crystalline phases are observed. The relative fraction of the crystalline phase governs the development of magnetic hyperfine fields in the residual amorphous matrix even if this was fully paramagnetic in the as-quenched state. The development of hyperfine interactions is discussed as a function of annealing temperature and composition of the investigated alloys. ⁵⁷Fe Mössbauer spectrometry was used as a principal analytical method. Additional information related to the structural arrangement is obtained from X-ray diffractometry. It is shown that in the as-quenched state, the relative fraction of magnetic hyperfine interactions increases as the amount of B rises. In partially crystalline samples, the contribution of magnetic hyperfine interactions inside the retained amorphous matrix increases with annealing temperature even though the relative fraction of amorphous magnetic regions decreases.     

Microstructure and magnetic properties of Fe72.5Cu1M2V2Si13.5B9 (M=Nb, Mo, (NbMo), (MoW)) nanocrystalline alloys

The microstructure and magnetic properties of Finemet-type Fe_72.5Cu₁M₂V₂Si_13.5B₉ (M=Nb, Mo, (NbMo), (MoW)) alloys have been systematically studied. Results show that the nanocrystalline alloy with M=NbMo has the smallest grain size of about 8 nm. The order of the effect of Nb, Mo and W additions in decreasing the α-Fe grain size in nanocrystalline alloys is Nb>Mo>W. The best DC soft magnetic properties are obtained in the alloy with M=Nb. In the case of AC soft magnetic properties, the Nb alloy also exhibits a very low core loss comparing with typical Finemet alloy. Therefore, the Nb alloy is suitable for use as a transformer core material. In addition, it is shown that a narrow grain size distribution and a uniform dispersion of α-Fe grains in the amorphous matrix are very crucial for the development of new Finemet-type nanocrystalline alloys with good soft magnetic properties.     

The influence of NiO addition on the magnetic properties of polycrystalline yttrium iron garnet

The influence of NiO addition on the magnetic properties of polycrystalline Y₃Fe₅O₁₂ is studied for the saturation magnetization, Curie temperature, initial magnetic permeability and ferromagnetic resonance line width. Dependence of saturation magnetization on NiO addition suggest that Ni²⁺ ions enter octahedral sites of the garnet lattice. Real part of the complex initial permeability versus temperature curves reveal the single phase for samples with NiO content. The absence of any additional peak in these curves and the invariance of Curie temperature suggest that NiO addition cannot alter the magneto-crystalline anisotropy of the material. Variations of initial permeability with NiO content are due to change of saturation magnetization and grain size of the materials. The ferromagnetic resonance line width varies linearly with the porosity of samples with NiO showing no anisotropy contribution in it.     

Investigation of the magnetic properties and magnetic structure parameters of nanocrystalline Fe<Subscript>79</Subscript>Zr<Subscript>10</Subscript>N<Subscript>11</Subscript> films

The magnetic properties (magnetization curve, ferromagnetic resonance spectrum) of nanocrystalline Fe₇₉Zr₁₀N₁₁ films obtained by RF magnetron sputtering with subsequent annealing were studied experimentally, along with the fundamental magnetic constants of these films (saturation magnetization M _S, local magnetic anisotropy energy K, and the exchange coupling constant A). The magnetic properties are discussed within the random magnetic model, which determines the correlation of the magnetic properties with the fundamental magnetic constants and nanostructure parameters (grain size, magnetic anisotropy, and correlation radius R _C). The exchange correlation length 2R _L for the film magnetic microstructure was determined by correlation magnetometry.