Studies of thin FeAlN films prepared by different techniques

The microstructure, morphology, and magnetic properties of FeAlN films deposited by reactive rf magnetron sputtering with subsequent treatment by three techniques, namely, in situ, ex situ (with the sputtering and annealing processes separated), and thermal crystallization of amorphous alloys, have been studied. FeAlN films prepared by the ex situ technique exhibit the best soft magnetic characteristics. Thermal crystallization of amorphous alloys produced films with properties having the highest thermal stability. Films 800-to 1000-nm thick were found to have the best soft magnetic properties. The dependences of the properties of FeAlN films on nitrogen content and annealing temperature were established. The conditions favoring the preparation of thin nanostructured FeAlN films featuring the best soft magnetic characteristics (saturation induction B _S = 1.8 T, coercivity H _C = 1.2 Oe, magnetic susceptibility μ₁ (1 MHz) = 3400) were determined.     

Effect of 3d transition metal substitution on microstructure and microwave absorption properties of FeSiB nanocrystalline flakes

Effect of 3d transition metal substitution (Co and Ni) is studied on microstructure and absorption properties of FeSiB flakes in GHz. Fe_78−xM_xSi₉B₁₃ (M=Co or Ni, x=0, 5, 10 and 15) nanocrystalline flakes with nanocrystal/amorphous two-phase structure were prepared by ball milling. Substitution decreases the nanocrystal size and affects microwave behavior both compositionally and structurally according to the substitution mechanism. Compositional influence is contributing to the change of intrinsic magnetization parameters; structural influence works on exchange coupling. Absorption band of Fe₇₈Si₉B₁₃ flakes shifts towards lower frequency by the substitution, and Fe₆₃Co₁₅Si₉B₁₃ absorber shows promising absorption at C-band.     

Soft magnetic properties of amorphous Fe52Co34Hf7B6Cu1 alloy treated by pulsed magnetic field and annealing

<正>The crystallization,microstructure,and soft magnetic properties of Fe₅₂Co₃₄Hf₇B₆Cu₁ alloy are studied.Amorphous Fe₅₂Co₃₄Hf₇B₆Cu₁ alloys are first treated by a pulsed magnetic field with a medium frequency,and then annealed at 100℃-400℃for 30 min in a vacuum.The rise in temperature during the treatment by a pulsed magnetic field is measured by a non-contact infrared thermometer.The soft magnetic properties of specimens are measured by a vibrating sample magnetometer（VSM）.The microstructure changes of specimens are observed by a Mossbauer spectroscopy and transmission electron microscope（TEM）.The results show the medium-frequency pulsating magnetic field will promote nanocrystallization of the amorphous alloy with a lower temperature rise.The nanocrystalline phase isα-Fe（Co） with bcc crystal structure,and the grain size is about 10 nm.After vacuum annealing at 100℃for 30 min,scattering nanocrystalline phases become more uniform,the coercive force and the saturation magnetization of the specimens are 41.98 A/m and 185.15 emu/g.     

Fe65B22Nd9Mo4 bulk nanocomposite permanent magnets produced by crystallizing amorphous precursors

The Fe₆₅B₂₂Nd₉Mo₄ nanocomposite permanent magnets in the form of a rectangular cross sectioned rod have been prepared by annealing the amorphous precursors. The thermal behavior, structure and magnetic properties of the magnets have been investigated by differential scanning calorimetry, X-ray diffractometry, electron microscopy and magnetometry techniques. The as-cast Fe₆₅B₂₂Nd₉Mo₄ alloy showed soft magnetic properties, which changed into magnetically hard after annealing. Results provoke that the magnetic properties of the alloy are sensitive to thermal processing conditions. The optimum hard magnetic properties with a remanence (B_r) of 0.56 T, coercivity (_iH_c) of 920.7 kA/m and maximum energy product (BH)_max of 50.15 kJ/m³ were achieved after annealing the alloy at 983 K for 10 min. The good magnetic properties of Fe₆₅B₂₂Nd₉Mo₄ magnets are ascribed to the exchange coupling between the nano-scaled soft α-Fe, Fe₃B and hard Nd₂Fe₁₄B magnetic grains.     

Influence of Al and Ni on the magnetic properties of Finemet alloys

Crystallization behavior and soft magnetic properties of the FeSiBCuNbM (M=Al or Ni) Finemet alloys are investigated by X-ray diffraction, differential scanning calorimetry, hysteresis loop tracer, and vibrating sample magnetometry. The nanocrystalline alloys are prepared by annealing melt-spun amorphous ribbons at different temperatures. Results indicate that the partial substitution of Ni or Al for Nb results in the increase of saturation magnetic induction density (B_s) of the alloys. The alloys with Al or Ni show favorable combination of soft magnetic properties. The partial substitution of Ni for Nb enhances the B_s value, while Al decreases coercivity. The mechanism underlining the magnetic behavior is discussed.     

Structural transformations and magnetic properties of Fe60Pt15B25 and Fe60Pt25B15 nanocomposite alloys

Structural and magnetic properties of two rapidly solidified and post-annealed Fe₆₀Pt₁₅B₂₅ and Fe₆₀Pt₂₅B₁₅ alloys are compared. The as-quenched Fe₆₀Pt₁₅B₂₅ ribbon was fully amorphous whereas in the Fe₆₀Pt₂₅B₁₅ alloy the amorphous phase coexists with an fcc FePt disordered solid solution. Differential scanning calorimetry curves of both alloys reveal a single exothermal peak with onset temperatures of 873 and 847 K for Fe₆₀Pt₁₅B₂₅ and Fe₆₀Pt₂₅B₁₅, respectively. Magnetically hard, tetragonal ordered L1₀ FePt and magnetically soft Fe₂B nanocrystalline phases were formed due to the annealing of the alloys, as indicated by X-ray diffraction and Mössbauer spectroscopy measurements. Two-phase behavior was detected in the temperature dependence of magnetization of the annealed samples. A magnetic hardening was observed for all annealed ribbons. Magnetic properties of the annealed alloys, studied by hysteresis loop measurements, were related to the differences in the relative fractions of the hard and soft magnetic phases calculated from Mössbauer spectra. The alloy with 25 at% Pt exhibits better hard magnetic properties (H_c=437 kA/m, M_r/M_s=0.74) than the alloy with smaller Pt content (H_c=270 kA/m, M_r/M_s=0.73) mainly due to the larger abundance of the ordered tetragonal FePt phase.     

Microstructure and soft magnetic properties of Finemet-type ribbons obtained by twin-roller melt-spinning

Soft magnetic ribbons of Finemet-type (Fe_73.5Cu₁Nb₃Si_13.5B₉) alloys are synthesized by the twin-roller melt-spinning technique directly from the melt, at tangential wheel speeds of 15, 18, 19 and 20 m/s. The microstructure and the magnetic properties are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), differential thermal analysis (DTA), thermo-gravimetric analysis (TGA) and hysteresis loops measurements. Samples cooled at 20 m/s are amorphous, while those quenched at lower wheel speeds are partially crystalline. All samples studied present saturation magnetization values (150-160 A m²/kg) higher than the commercial Finemet alloys (∼135 A m²/kg), obtained by controlled crystallization of amorphous single-roller melt-spun alloys. Optimal soft magnetic properties - σ_S=(154±8) A m²/kg and H_C=(6.9±0.9) A/m - are found in samples quenched at 19 m/s, consisting of size-distributed bcc Fe-Si nanograins (∼18 nm in average) embedded in an amorphous residual matrix. A minority nanocrystalline magnetic phase (≤10 nm) is also detected.     

Development of soft magnetic amorphous alloys with distinctly high Fe content

This paper reports on the preparation of Fe_(82.7-85.7)Si_(2-4.9)B_(9.2-11.2)P_(1.5-2.7)C_(0.8) soft magnetic amorphous alloys with a distinctly high Fe content of 93.5-95.5 wt.% by component design and composition adjustment. All alloys can be readily fabricated into completely amorphous ribbon samples with good surface quality by the single copper roller melt-spinning method. These alloys show good bending ductility and excellent magnetic properties after annealing, i.e., low coercivity(H_c) of 3.3-5.9 A/m, high permeability(μ_e)of 5000-10000 and high flux saturation density(B_s) of 1.63-1.66 T. The mechanism of the good glass forming ability(GFA) and soft-magnetic properties are explored. The amorphous alloys with the high Fe content comparable to that of the desired high Si alloy can be promising candidates for the potential application in electric devices.     

Effect of compositional variation on the soft magnetic properties of Fe(87−x−y)CoxTi7 Zr6By amorphous ribbons

The effect of the replacement of Fe by Co or B on the thermal stability and soft magnetic properties of the Fe-based amorphous metallic ribbons with Fe_(87−x−y)Co_xTi₇Zr₆B_y (x = 10, 20% and y = 8, 10, 12%) produced by melt-spinning technique was investigated. For the melt-spun amorphous ribbons, the values of saturation magnetization and coercivity were observed to range from 107.00 to 152.38 emu/g and from 0.012 to 0.446 Oe, respectively. The thermal properties such as T_g, T_x, and ΔT_x were in the range of 796.7–809.6 K, 840.2–853.5 K, and 35.8–54.5 K, respectively. In the Fe–Co–Ti–Zr–B alloys, the Co substitution for Fe improved the soft magnetic properties but decreased the thermal stability. For magnetic properties, the coercivity (H_c) decreased and saturation magnetization (M_s) increased by the addition of Co. However, the supercooled liquid region (ΔT_x) decreased by the addition of Co. Meanwhile, the B substitution for Fe had no meaningful change on the thermal stability and soft magnetic properties. The amorphous ribbon of Fe₅₉Co₂₀Ti₇Zr₆B₈ exhibited the best soft magnetic properties such as the low coercivity of 0.025 Oe and the high saturation magnetization of 152.38 emu/g.     

Effect of niobium on microstructure and magnetic properties of bulk anisotropic NdFeB/α-Fe nanocomposites

Bulk anisotropic NdFeB/α-Fe nano-composites were obtained directly from alloys of Nd₁₁Dy_0.5Fe_82.4−xNb_xB_6.1 (x=0,0.5,1.0,1.5). High resolution transmission electron microscopy images showed the existence of Nb-rich amorphous grain boundary phase in the alloys with Nb doped. Field emission scanning electron microscope morphologies and X-ray diffraction patterns revealed the grain size and grain alignment of hot pressed and hot deformed nanocomposites. It was found that Nb could refine the grain size and grain texture in hot worked ribbons. Vibrating sample magnetometer results showed that the magnetic properties of the anisotropic nanocomposites were improved with increased Nb doping. The remanence, coercivity and maximum energy product of the bulk anisotropic Nd₁₁Dy_0.5Fe_80.4Nb₂B_6.1 nanocomposites were 1.04 T, 563 kA/m and 146 kJ/m³, respectively.     

Effects of In-substitution on the microstructure and magnetic properties of Bi-CVG ferrite with low temperature sintering

[Y_1.05Bi_0.75Ca_1.2](Fe_4.4−xIn_xV_0.6)O₁₂(In_x:Bi-CVG) ferrite material has been prepared successfully by a solid-state reaction method. The effects of In³⁺ substitution and sintering temperatures on the bulk density, microstructure and magnetic properties are performed by X-ray diffraction (XRD), scanning electron microscopy (SEM), materials automatic test system (MATS) and microwave ferrite parameters meter. The results show that In³⁺ can lower the sintering temperatures and enhance the magnetic properties of Bi-CVG ferrite. Besides, all sintered specimens with different In³⁺ contents show a single garnet crystal structure. The specimen of [Y_1.05Bi_0.75Ca_1.2](Fe₄In_0.4V_0.6)O₁₂ sintered at 1075 °C shows homogenous distribution of grain size and densified microstructures. The ferromagnetic resonance linewidth (ΔH) has an increase with In³⁺ contents. Additionally, the sample has the optimum magnetic properties: ρ=5.23 g/cm³, B_r=31.3 mT, H_c=378.8 A/m, 4πM_s=506.2×10⁻⁴ T.     

Preparation, and magnetic and electromagnetic properties of La-doped strontium ferrite films

SrLa_xFe_12−xO₁₉ films (x=0-1.0) with large magneto-crystalline anisotropy were synthesized on SiO₂ substrate by sol-gel and self-propagating high-temperature synthesis technique. The films were characterized by various experimental techniques including X-ray diffraction analysis, Field Emission Scanning Electron Microscope, Atomic Force Microscopy, Vibrating Sample Magnetometry and vector network analyzer. The results show that La ions completely enter into strontium ferrite lattice without changing the ferrite appearance; its grain size is approximately 40-80 nm, its length is 100 nm; the magnetoplumbite structure is proved through testing a concertina form of the crystal grain; the maximum coercivity is 5986 Oe at x=0.2; La-doped films possess a wider microwave absorption frequency range with better gross loss angle tangent (tan δ>0.1), from 9 to 10.5 GHz at x=0.2, where the maximum value of tan δ reaches 0.2709. The La-doped films reach smaller nanometer size, better magnetic properties and microwave absorption properties with the doping of lanthanum.     

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.     

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.     

New Fe-based amorphous compound powder cores with superior DC-bias properties and low loss characteristics

The Fe–Si–B–P–C metallic glassy alloys exhibit relatively high glass forming ability (GFA) as well as good soft magnetic properties such as ultra-low core loss. In this paper, the metallic glassy alloy (Fe_0.76Si_0.09B_0.10P_0.05)₉₈C₂ has been newly developed. A new Fe-based amorphous compound powder was prepared from FeSiB amorphous powder by crushing the amorphous ribbons as the first magnetic component and FeSiBPC metallic glassy powder by water atomization as the second magnetic component. Subsequently by adding organic and inorganic binders to the compound powder and cold pressing, the new Fe-based amorphous compound powder cores were fabricated. These new Fe-based amorphous compound powder cores combine the superior DC-bias properties and the excellently low core loss. The core loss of 453 kW/m³ at B_m=0.1 T and f=100 kHz was obtained when the mass ratio of FeSiB/FeSiBPC equals 3:2, and meanwhile the DC-bias properties of the new Fe-based amorphous compound powder cores just increased by 10% at H=100 Oe for μ=60 compared to those of the FeSiBPC powder cores. In addition, with the increase in the content of the FeSiPC metallic glassy powder, the core loss tends to decrease.     

The effect of B2O3 addition to the microstructure and magnetic properties of Ni0.4Zn0.6Fe2O4 ferrite

The effects of 0.01 and 0.1 mol B₂O₃ addition to the microstructure and magnetic properties of a Ni–Zn ferrite composition expressed by a molecular formula of Ni_0.4Zn_0.6Fe₂O₄ were investigated. The toroid-shaped samples prepared by pressing the milled raw materials used in the preparation of the composition were sintered in the range of 1000–1300 °C. The addition of 0.01 mol B₂O₃ increased the grain growth and densification giving rise to reduced intergranular and intragranular porosity due to liquid-phase sintering. The sintered toroid sample at 1300 °C gave the optimum magnetic properties of B_r=170 mT, H_c=0.025 kA/m and a high initial permeability value of μ_i=4000. The increment of the B₂O₃ content to 0.1 mol resulted in a pronounced grain growth and also gave rise to large porosity due to the evaporation of B₂O₃ at higher sintering temperatures. Hence, it resulted in an air-gap effect in the hysteresis curves of these samples.     

First-principle study of the structural, electronic, and magnetic properties of amorphous Fe-B alloys

The structural, electronic, and magnetic properties of amorphous Fe_100−xB_x alloys (x=9, 17, 25, 27.3, 33.3, 36.3) are investigated using first-principles calculations. In these amorphous alloys, the short-range order is manifested as a series of Fe- or B-centered polyhedra such as tricapped trigonal prism, icosahedron, and bcc-like structural unit. The electron densities of states of the amorphous alloys resemble those of crystalline Fe borides, which further confirm the similarity of the local order in the amorphous and crystalline phases. All B atoms carry small negative moments of about −0.1μ_B, while small negative moments are also found on very few Fe sites for the Fe-rich compositions (x=9, 17). The average magnetic moment per Fe atom decreases nonlinearly with increasing B composition, which can be associated with the nonlinear relationship between mass density and composition.     

Preparation and characterization of ZnSn-substituted barium ferrite thin films

The preparation of ZnSn-substituted barium ferrite films by sputtering deposition was studied. The as-sputtered films were amorphous, and annealing at a minimum of 750 °C was required to crystallize the films, based on the X-ray diffraction analysis and the magnetic measurements. Scanning electron microscopy combined with energy-dispersive X-ray spectroscopic microanalysis confirmed that the films were single phase with the composition BaZn_xSn_xFe_12−2xO₁₉, x=0.2−0.3, and their thicknesses were 0.4-1.0 μm when annealed at 750-900 °C. Atomic and magnetic force microscopy studies showed no significant grain growth upon annealing and that the films consisted of single-domain grains forming interaction-cluster-type domains. The natural ferromagnetic resonance frequency was determined at around 4 GHz, together with substantial magnetic losses that make these films promising candidates for microwave absorbers.     

Nanocrystallisation of an Fe44.5Co44.5Zr7B4 amorphous magnetic alloy

The crystallisation of amorphous Fe_44.5Co_44.5Zr₇B₄ was investigated using DSC, electrical resistivity, TEM, HRTEM, CBED and VSM. Melt-spun amorphous Fe_44.5Co_44.5Zr₇B₄ crystallised by the primary crystallisation mode: the DSC results showed two exothermal peaks during heating. The electrical resistivity dropped sharply during the crystallisation event, which was consistent with DSC characterisation. From TEM, HRTEM and CBED results, primary crystallisation products which appeared to be clusters of crystals were found to be single crystal precipitates; these crystals formed in a compact dendritic morphology. Direct measurement of nucleation density and volume fraction was carried out using TEM analysis. The nucleation density was found to be high even in the absence of copper addition. The crystal growth was slow when the average size reached around 30?nm; this resulted in a stable nanocrystalline structure. The soft magnetic properties were improved after nanocrystallisation, the magnetic properties were related to the crystalline volume fraction and the Herzer model.     

Annealing temperature effect on microstructure,magnetic and microwave properties of Fe-based amorphous alloy powders

Fe₇₄Ni₃Si₁₃Cr₆W₄ amorphous alloy powders were annealed at different temperature (T) for 1.5 h to fabricate the corresponding amorphous and nanocrystalline powders. The influences of T on the crystalline structure, morphology, magnetic and microwave electromagnetic properties of the resultant samples were investigated via X-ray diffraction, scanning electron microscopy, vibrating sample magnetometer and vector network analyzer. The results show that the powder samples obtained at T of 650 °C or more are composed of lots of ultra-fine α-Fe(Si) grains embedded in an amorphous matrix. When T increases from 350 to 750 °C, the saturated magnetization and coercivity of the as-annealed powder samples both increase monotonously whereas the relative real permittivity shows a minimal value and the relative real permeability shows a maximal value at T of 650 °C. Thus the powder samples annealed at 650 °C show optimal reflection loss under −10 dB in the whole C-band. These results here suggest that the annealing heat treatment of Fe-based amorphous alloy is an effective approach to fabricate high performance microwave absorber with reasonable permittivity and large permeability simultaneously via adjusting T.