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.     

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.     

Effect of Mn on the magnetic properties of Fe3B/Nd2Fe14B nanocomposites

The magnetic properties of Nd_4.5Fe_77−xMn_xB_18.5 (x=0, 1 and 2) nanocomposites prepared by the crystallization of amorphous precursors were investigated. Addition of Mn is found to decrease the crystallization temperature of the amorphous ribbons. The intrinsic coercivity _iH_c and maximum energy product (BH)_max increase from 2.6 kOe and 9.1 MGOe for x=0 to 3.1 kOe and 10.3 MGOe for x=1, respectively, and the remanence ratio M_r/M_s increases from 0.70 to 0.72. The effect of Mn on Curie temperature T_C and the thermal stability of M_r and _iH_c were also studied. ⁵⁷Fe Mössbauer spectra have been recorded for x=0, 1 and 2 ribbons at room temperature and site preference of the Mn atoms in Fe₃B and Nd₂Fe₁₄B phases is discussed using the Mössbauer spectroscopy.     

Influence of heating rate on the crystalline properties of 0.7BiFeO3-0.3PbTiO3 thin films prepared by sol-gel process

0.7BiFeO₃-0.3PbTiO₃ (BFPT7030) thin films were deposited on SiO₂/Si substrates by sol-gel process. The influence of heating rate on the crystalline properties of BFPT7030 thin films were studied by X-ray diffraction (XRD), scanning electron microscope (SEM), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). XRD patterns of the films showed that a pure perovskite phase exists in BFPT7030 films annealed by rapid thermal annealing (RTA) technique. SEM and AFM observations demonstrated that the BFPT7030 films annealed by RTA at 700 °C for 90 s with the heating rate of 1 °C s⁻¹ could show a dense, crack-free surface morphology, and the films’ grains grow better than those of the films annealed by RTA at the same temperature with other heating rates. XPS results of the films indicated that the ratio of Fe³⁺:Fe²⁺ is about 21:10 and 9:5 for the films annealed by RTA at 700 °C for 90 s with the heating rate of 1 and 20 °C s⁻¹, respectively. That means the higher the heating rate, the higher the concentration of Fe²⁺ in the BFPT7030 thin films.     

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.     

Magnetic and electrical properties of bulk BaTiO3+MgFe2O4 composite

BaTiO₃+MgFe₂O₄ material system was synthesized by hybrid chemical process using chlorides and nitrates of barium, titanium, iron, and magnesium. Magnetic properties of the composite samples measured as a function of annealing conditions indicated soft magnetic behavior. Saturation specific magnetization from 8 21 emu/g was observed for samples annealed at temperature between 950 and 1150 °C. Variation of specific saturation magnetization with respect to annealing temperature was related with the distribution of Fe cations in the tetrahedral and octahedral sites of MgFe₂O₄. Electrical properties of the samples annealed at different temperatures were measured to analyze the coexistence of ferroelectric phase. Dielectric constant varying from 15 to 200 with respect to frequency was observed for samples annealed from 950 to 1150 °C.     

Thermal annealing effects on the magnetic behavior of Ce2NiSi3

We have investigated the crystallographic, magnetic and thermodynamic properties of the as-cast and annealed Ce₂NiSi₃ alloys, crystallizing in the AlB₂-type hexagonal structure. The DC-magnetic susceptibility data show that the as-cast sample exhibits an antiferromagnetic (AFM) ordering below T_N= 3.8 K, whereas the annealed sample shows, at 4.2 K, a magnetic transition of AFM nature and, around 2.5 K, an additional anomaly. The specific heat shows a peak with at 3.8 K for the as cast sample, which shifts to lower temperatures when the magnetic field increases, consistent with the antiferromagnetic nature of the transition. On the other hand, in the annealed alloy, the maximum of the specific heat peak reaches at 4.2 K, and no additional anomalies were observed. The different magnetic behavior between the as-cast and annealed samples is attributed to thermal effects on the structural disorder of nickel and silicon atoms, as already observed in other isotypic R₂TSi₃ alloys, where R=U or Ce, and T= transition metal.     

Effect of annealing on magnetoimpedance of Co68Fe4Zr10Cu2B16 ribbons

Magnetoimpedance (MI) in Co₆₈Fe₄Zr₁₀Cu₂B₁₆ alloy has been investigated in the frequency range 500 kHz–5 MHz and with the application of external steady magnetic field in the longitudinal direction, up to 100 Oe. MI measurements were carried out on as-cast ribbons and also on conventionally annealed and Joule-annealed ribbons. In as cast ribbons, the maximum MI observed is 13% at a frequency of 500 kHz and it decreases to 5% and 4% with conventional annealing at 100 °C and 150 °C, respectively. On the other hand, MI decreases to 8% and 6% with Joule annealing employing currents of 100 mA and 200 mA, respectively. However, Joule annealing with the application of a magnetic field of 5–10 Oe in the transverse direction causes the MI to decrease to 12% and 11% for currents of 100 mA and 200 mA, respectively. In the as-cast ribbons, double peak behavior is observed in all the frequencies whereas, in the annealed ribbons, double peak behavior in general is observed only at high frequencies.     

Synthesis,structures and magnetic properties of Pr-lean Pr2Fe14B/Fe3B nanocomposite alloys

The lean rare-earth Pr_4.5Fe_77−xTi_xB_18.5 (x=0, 1, 4, 5) nanocomposite alloys were prepared by melt spinning method and subsequent thermal annealing. The effect of Ti content and annealing temperature on the magnetic properties and the microstructure of these magnets were investigated. The enhancing coercivity H_c from 211.4 to 338.2 kA/m has been observed at the optimal annealing temperature of 700 °C by the addition of 5 at% Ti in Pr₂Fe₁₄B/Fe₃B alloys. It was also found that increasing Ti content leads to marked grain refinement in the annealed alloys, resulting in strong exchange-coupling interaction between the hard and the soft phases in these ribbons. In addition, the magnetization reversal behaviors of Pr₂Fe₁₄B/Fe₃B nanocomposites were discussed in detail.     

Effect of nanoscale thin films of Dy2Fe14B on the magnetic hysteresis characteristics of melt-spun ribbons of Nd2Fe14B

The effectiveness of nanoscale Dy₂Fe₁₄B thin films on coercivity and energy product of melt-spun ribbons of Nd₂Fe₁₄B at high temperatures was investigated. It is hypothesized that the nanoscale Dy-thin film will act as an obstacle for the nucleation of reverse domains and also maximize the energy of domain walls and thereby improve the magnetic performance at high temperatures. Pulsed laser deposition (PLD) of amorphous Dy₂Fe₁₄B layers on Nd₂Fe₁₄B melt-spun ribbons was performed for a nominal thickness of 40 nm. The coated ribbons were then annealed in environmentally controlled quartz furnace at two different cycles (750 °C for 15 min and 900 °C for 2 h) to cause crystallization. Magnetic hysteresis tests conducted at 300 and 400 K revealed that there is small but consistent improvement in the magnetic properties of the coated ribbons annealed at 750 °C for 15 min. However, higher temperature annealing (900 °C for 2 h) drastically reduced the magnetic properties. The incomplete recrystallization of amorphous structure at 750 °C for 15 min and large grain growth and formation of non-magnetic phases at 900 °C for 2 h are believed to be responsible for not meeting the expected magnetic performance.     

Magnetic properties of Nd0.9Dy0.1Fe3(BO3)4

The magnetic properties of trigonal Nd_0.9Dy_0.1Fe₃(BO₃)₄ substituted compound with the competitive Nd-Fe and Dy-Fe exchange interactions have been investigated. It has been shown that in Nd_0.9Dy_0.1Fe₃(BO₃)₄ a spontaneous spin-reorientation transition from an ease-axis state to an easy-plane occurs near 8 K. Anomalies of the magnetization curves are observed in a spin-flop transition induced by the magnetic field B‖c. The calculations were performed using a molecular-field approximation and a crystal-field model for the rare-earth subsystem. Extensive experimental data on the magnetic properties of Nd_0.9Dy_0.1Fe₃(BO₃)₄ have been interpreted and good agreement between theory and experiment has been achieved using the obtained theoretical dependences.     

Research on preparing compact bulk nanocomposite Nd2Fe14B/α-Fe magnetic materials by hot extrusion

In this paper, compact bulk nanocomposite Nd₂Fe₁₄B/α-Fe magnetic materials were prepared by hot extrusion of amorphous and nanocrystalline powders, which were prepared by high-energy ball-milling (HEBM) of the Nd₂Fe₁₄ B-type hard magnetic phase with 20 vol% of α-Fe as soft magnetic phase. The extrusion temperature has important influence on magnetic properties and microstructure of magnetic materials. The results show that the grain size of Nd₂Fe₁₄B and α-Fe phase increases steadily with increasing extrusion temperature. Furthermore, optimal extrusion temperature of 1223 K occurs, at which the highest magnetic properties and relative density can be obtained.     

High temperature ferromagnetism of the vacuum-annealed (In1−xFex)2O3 powders

(In_1−xFe_x)₂O₃ (x = 0.02, 0.05, 0.2) powders were prepared by a solid state reaction method and a vacuum annealing process. A systematic study was done on the structural and magnetic properties of (In_1−xFe_x)₂O₃ powders as a function of Fe concentration and annealing temperature. The X-ray diffraction and high-resolution transmission electron microscopy results confirmed that there were not any Fe or Fe oxide secondary phases in vacuum-annealed (In_1−xFe_x)₂O₃ samples and the Fe element was incorporated into the indium oxide lattice by substituting the position of indium atoms. The X-ray photoelectron spectroscopy revealed that both Fe²⁺ and Fe³⁺ ions existed in the samples. Magnetic measurements indicated that all samples were ferromagnetic with the magnetic moment of 0.49-1.73 μ_B/Fe and the Curie temperature around 783 K. The appearance of ferromagnetism was attributed to the ferromagnetic coupling of Fe²⁺ and Fe³⁺ ions via an electron trapped in a bridging oxygen vacancy.     

High-throughput characterization of BixY3−xFe5O12 combinatorial thin films by magneto-optical imaging technique

Bi_xY_3−xFe₅O₁₂ thin films have been grown on GGG (Gd₃Ga₅O₁₂) (1 1 1) substrates by the combinatorial composition-spread techniques under substrate temperature (T_sub) ranging from 410 to 700 °C and O₂ pressure of 200 mTorr. In order to study the effect of substrates on the deposition of Bi_xY_3−xFe₅O₁₂ thin films, garnet substrates annealed at 1300 °C for 3 h were also used. Magneto-optical properties were characterized by our home-designed magneto-optical imaging system. From the maps of Faraday rotation angle θ_F, it was evident that the Faraday effect appears only when T_sub = 430-630 °C. θ_F reaches to the maximum value (∼6°/μm, λ = 632 nm) at 500 °C, and is proportional to the Bi contents. XRD and EPMA analyses showed that Bi ions are easier to substitute for Y sites and better crystallinity is obtained for annealed substrates than for commercial ones.     

Enhanced alignment and magnetic properties of die-upset nano-crystal Nd2Fe14B magnets with Nb addition

It is difficult to obtain the crystallographic alignment for stoichiometric Nd₂Fe₁₄B alloys by applying the melt-spun and subsequent hot-pressing and hot-deformation techniques. However, the enhanced alignment and magnetic properties of die-upset nano-crystal Nd₂Fe₁₄B magnets have been obtained by Nb addition in the present paper. The magnetic properties studies show that Nb addition leads to the remarkable increase of remanence B_r and intrinsic coercivity H_ci, which is due to the improvement of c-axis texture and refinement of microstructure. Microstructure studies using transmission electron microscopy (TEM) and X-ray diffraction (XRD) reveal that Nb atoms are enriched at grain boundary and the NbFeB phase is observed with increasing Nb content. Since some Fe atoms in the Nd₂Fe₁₄B phase participate in the formation of NbFeB phase, the excessive Nd atoms may be enriched at grain boundary, which may improve the physical property of grain boundary and provide a mass transport pass for preferential growth of oriented Nd₂Fe₁₄B grains, thus leading to the enhanced alignment and magnetic properties.     

The effect of different temperature annealing on phase relation of LaFe11.5Si1.5 and the magnetocaloric effects of La0.8Ce0.2Fe11.5−xCoxSi1.5 alloys

The phase relation of LaFe_11.5Si_1.5 alloys annealed at different high-temperature from 1223 K (5 h) to 1673 K (0.5 h) has been studied. The powder X-ray diffraction (XRD) patterns show that large amount of 1:13 phase begins to form in the matrix alloy consisting of α-Fe and LaFeSi phases when the annealing temperature is 1423 K. In the temperature range from 1423  to 1523 K, α-Fe and LaFeSi phases rapidly decrease to form 1:13 phase, and LaFeSi phase is rarely observed in the XRD pattern of LaFe_11.5Si_1.5 alloy annealed at 1523 K. With annealing temperature increasing from 1573  to 1673 K, the LaFeSi phase is detected again in the LaFe_11.5Si_1.5 alloy, and there is La₅Si₃ phase when the annealing temperature reaches 1673 K. There almost is no change in the XRD patterns of LaFe_11.5Si_1.5 alloys annealed at 1523 K for 3-5 h. According to this result, the La_0.8Ce_0.2Fe_11.5−xCo_xSi_1.5 (0≤×≤0.7) alloys are annealed at 1523 K (3 h). The analysis of XRD patterns shows that La_0.8Ce_0.2Fe_11.5xCo_xSi_1.5 alloys consist of the NaZn₁₃-type main phase and α-Fe impurity phase. With the increase of Co content from x=0 to 0.7, the Curie temperature T_C increases from 180 to 266 K. Because the increase of Co content can weaken the itinerant electron metamagnetic transition, the order of the magnetic transition at T_C changes from first to second-order between x=0.3 and 0.5. Although the magnetic entropy change decreases from 34.9 to 6.8 J/kg K with increasing Co concentration at a low magnetic field of 0-2 T, the thermal and magnetic hysteresis loss reduces remarkably, which is very important for the magnetic refrigerant near room temperature.     

Improvement of the magnetic properties of Nd9.5Fe81Zr3B6.5 nanocomposite magnets by semi-melt spinning

Nd_9.5Fe₈₁Zr₃B_6.5 ribbons are prepared by single roller melt-spinning technique at 1150 °C which is in the solid and liquid coexistence zone. The phase evolution and magnetic properties were studied by X-ray diffraction, differential scanning calorimetry, transmission electron microscopy observations, and magnetization measurements. The experimental results show that in comparison to the ribbons quenching at higher temperature, the thickness of ribbons prepared at 1150 °C are insensitive to the wheel speed and an uniform nanoscale structure with fine grains can be obtained directly from the semi-melt and the exchange coupling interaction between the grains was enhanced for the nanocomposite permanent alloy which can contributed to excellent magnetic properties.     

Effects of forming gas annealing on LiNbO3 single crystals

Z-cut congruent LiNbO₃ single crystals were annealed in 95%N₂+5%H₂ at high temperatures. X-ray diffraction showed that 2θ of (0 0 0 6) peak is obviously reduced by 0.6° and 1.0° for the samples annealed at 600 and 900 °C, respectively. A new peak appears at the high-energy side of O 1s spectrum in X-ray photoelelectron spectroscopy (XPS) analyses, and the leakage current is greatly increased. It is proposed that hydrogen is incorporated in LiNbO₃ single crystals through forming gas annealing at temperatures up to 900 °C and exists in LiNbO₃ as a proton bound to an oxygen ion through O-H bond with its electron donated.     

X-ray photoelectron spectroscopic investigations on cubic BaTiO3, BaTi0.9Fe0.1O3 and Ba0.9Nd0.1TiO3 systems

X-ray photoelectron spectroscopic (XPS) studies were carried out on wet-chemically synthesized cubic BaTiO₃, Ba_0.9Nd_0.1TiO₃ and BaTi_0.9Fe_0.1O_3−δ powders. The compounds were prepared by hydrothermal and gel to crystallite conversion technique; and phases formed readily at 420 K. The phase purity of the powders was confirmed from X-ray diffractometry. Chemical state and chemical environment of the constituent elements in the compositions were examined by XPS. Ba²⁺ was found to exist in two different chemical environments in these titanates. The Ti 2p_3/2 photoelectron peak in BaTi_0.9Fe_0.1O_3−δ was found to be broadened after Fe³⁺ substitution. Any resolvable broadening was not observed distinctly in the Ti 2p peak for Ba_0.9Nd_0.1TiO₃, unsintered BaTiO₃ and BaTiO₃ annealed in hydrogen (8% H₂ + Ar) at 1000 K. The prevalence of mixed-valent titanium and iron in BaTi_0.9Fe_0.1O_3−δ composition was evident from the XPS results and was further supported by the enhanced electrical conductivity at 298-550 K for BaTi_0.9Fe_0.1O_3−δ in comparison to BaTiO₃ and Ba_0.9Nd_0.1TiO₃. Hydroxyl incorporation was facilitated by substituting Nd³⁺ in Ba-sublattice. The presence of hydroxyls was observed from the broadening of the O 1s peak in XPS studies of the compounds.     

Magnetic properties enhancement of Nd2Fe14B/α-Fe nanocomposites by Ta substitution

Nanostructured Nd_9.5Fe_84−xB_6.5Ta_x (x=0, 0.5, 1, 1.5, and 2) ribbons composed of Nd₂Fe₁₄B and α-Fe phases with a high coercivity and maximum energy product are fabricated by direct melt spinning. The effects of Ta addition on the structures and magnetic properties of melt-spun Nd_9.5Fe_84−xB_6.5Ta_x (x=0, 0.5, 1, 1.5, and 2) ribbons have been investigated. Compared with addition-free ribbons, small addition of Ta is found to reduce the grain sizes of the samples and improve their magnetic properties due to a strong exchange coupling between the Nd₂Fe₁₄B hard phase and α-Fe soft phase. A coercive field of 750 kA/m and a maximum energy product of 158 kJ/m³ in melt-spun Nd_9.5Fe_82.5B_6.5Ta_1.5 ribbons are obtained at room temperature.