Research on the magnetic properties and crystal lattice aberrance of melt-spun Nd9Fe85−xMnxB6 (x=0–1)

Magnetic properties and crystal lattice aberrance of melt-spun Nd₉Fe_85−xMn_xB₆ (x=0,0.5,1) nanocomposite materials were investigated by DTA, XRD, EXAFS and VSM. It was found that a certain amount of manganese added to Nd₉Fe₈₅B₆ magnets can promote crystal and enhances the hard magnetic properties. The coercivity and remanence ratio increases from 4.3 kOe and 0.70 to 5.0 kOe and 0.72, respectively. The remain magnetization has not distinct reduce under the optimum annealing method. M–T shows Mn doping decreases the Curie temperature of the Nd₂Fe₁₄B phase and raises that of α-Fe phase. The origin for the enhancement of magnetic properties is not only related to the reduction of grain size which enhances the exchange coupling between grains but also to the precise crystal structure.     

Mössbauer study of intergranular phase in Nd 8 Fe86 − x Nb x B6(x = 0, 1, 2, 3) nanocomposite magnet

Nd₈Fe_86???x Nb _x B₆ (x = 0, 1, 2, 3) nanocomposite magnet has been studied by Mössbauer spectroscopy and nanostructure observation. It was found that intergranular phase formed between α-Fe and Nd₂Fe₁₄B phase in NdFeNbB alloys plays a significant role on the magnetic properties. By the addition of Nb into Nd₈Fe₈₆B₆ composition, coercivity was found to increase by 25% due to the grain refinement of both the soft and hard magnetic phases which was decreased from 50 nm of virgin Nd₈Fe₈₆B₆ to 25 nm in Nd₈Fe₈₅Nb₁B₆ alloys. The role of Nb addition was confirmed to stabilize the Nd₂Fe₁₄B lattice preventing from thermal vibration of the corresponding sites at where Fe atoms are substituted by Nb in the Nd₂Fe₁₄B lattice. The enhanced coercivity was originated from the exchange hardening of soft and amorphous phases surrounding the hard magnetic Nd₂Fe₁₄B crystal.     

快淬Nd3.6Pr5.4Fe83Co3B5薄带的反磁化行为和磁黏滞性

用电弧熔炼法制备了Nd_3.6Pr_5.4Fe₈₃Co₃B₅合金铸锭,然后利用熔旋快淬法在铜辊转速V=20m/s下制备了Nd_3.6Pr_5.4Fe₈₃Co₃B₅薄带.快淬带主要由软磁相α-Fe和Nd₂Fe₁₄B型的硬磁相组成.采用直流退磁剩磁曲线方法分析了样品在反磁化过程中的可逆与不可逆磁化部分,并研究了软磁相和硬磁相的反磁化行为,得到样品的不可逆磁化形核场H_no约为440kA/m.同时研究了样品的磁黏滞性,结果表明由于软磁相的存在使得热激活体积较大. 关键词：     

Exchange coupling and remanence enhancement in nanocomposite Nd–Fe–B/FeCo multilayer films

Nd–Fe–B-type hard phase single layer films and nanocomposite Nd₂₈Fe₆₆B₆/Fe₅₀Co₅₀ multilayer films with Mo underlayers and overlayers have been fabricated on Si substrates by rf sputtering. The hysteresis loops of all films indicated simple single loops for fixed Nd–Fe–B layer thickness (10 nm) and different FeCo layer thickness (d_FeCo=1–50 nm). The remanence of these films is found to increase with increasing d_FeCo and the coercivity decrease with increasing d_FeCo. It is shown that high remanence is achieved in the nanocomposite multilayer films consisting of the hard magnetic Nd–Fe–B-type phase and soft magnetic phase FeCo with 20 nm?d_FeCo?3 nm. The sample of maximum energy product is 27 MG Oe for d_FeCo=5 nm at room temperature. The enhancement of the remanence and energy products in nanocomposite multilayer films is attributed to the exchange coupling between the magnetically soft and hard phases.     

Nano-sized disorders in hard magnetic grains and their influence on magnetization reversal at artificial Nd/Nd2Fe14B interfaces

We have investigated the effect of lattice disorders near the surface of hard magnetic Nd₂Fe₁₄B grains on coercivity using artificial interfaces created by sputter depositing Nd on polished surface of Nd-Fe-B sintered magnets. The interfacial structure was manipulated by annealing the coated samples at 550 °C in vacuum with and without Ta cap. Nano-beam electron diffraction revealed a few nm thick disordered layer within the Nd₂Fe₁₄B phase at the Nd/Nd₂Fe₁₄B interface of a low coercivity sample, while a high coercivity sample showed a well-defined crystal structure of Nd₂Fe₁₄B near the NdO_x/Nd₂Fe₁₄B interface.     

相分布和晶粒尺寸对Nd2Fe14B/ɑ-Fe纳米复合永磁材料矫顽力的影响

本文采用统计平均方法研究了软、硬磁性晶粒尺寸及相分布对Nd2Fe14B/α-Fe纳米复合永磁材料矫顽力的影响。计算结果表明：对于单相纳米硬磁材料，磁体矫顽力随着硬磁性晶粒尺寸的减小而降低；对于软、硬两磁性相组成的Nd2Fe14B/a-Fe纳米复合永磁材料，两相的随机分布将导致磁体矫顽力随硬磁性晶粒尺寸的减小呈现极大值。本文的计算结果还表明当硬磁性晶粒尺寸大于软磁性晶粒的最佳尺寸时(15nm)，具有多层膜结构的Nd2Fe14B/a-Fe纳米复合永磁材料将比两相随机分布时具有更大的矫顽力。     

Magnetic properties and phase compositions of rapidly quenched Nd4Fe96−x B x after crystallization

Permanent magnets, composition Nd₄Fe_96?x B _x (x=10–21), were made by rapid quenching followed by crystallization. The effects of B concentration and annealing time on the magnetic properties and phase compositions were studied by Mössbauer spectroscopy and magnetic measurements. The stripping method was adopted to obtain the subspectral area of each Fe phase. Optimum magnetic properties are obtained for the composition Nd₄Fe₇₇B₁₉ annealed at 670°C for 3 minutes. Then the remanence is 12.0 kGs, the intrinsic coercivity 3.2 kOe, and the maximum energy product 12.6 MGOe. The crystalline phases are Fe₃B, Nd₂Fe₁₄B and α-Fe with volume percentages of 60%, 36%, and 4%, respectively.     

Ultra-fine grained Nd–Fe–B by high pressure reactive milling and desorption

This paper reports on the grain refinement in dynamic hydrogenation disproportionation desorption and recombination (d-HDDR) processed Nd-rich Nd₂Fe₁₄B and stoichiometric Nd₂Fe₁₄B powders using high pressure reactive milling (HPRM) followed by a subsequent desorption and recombination. In contrast to the dynamic-HDDR processed anisotropic powder with a grain size of the Nd₂Fe₁₄B phase of 300 nm, the new approach yields a further reduction of the Nd₂Fe₁₄B₁ grain size to less than 70 nm. Nd-rich Nd₂Fe₁₄B powder produced by HPRM and subsequent desorption exhibits a coercivity μ_0iH_c=1.35 T and a remanence of 0.80 T. In the stoichiometric material, the reduction of the Nd-content leads to an increase in remanence to 0.85 T. Additionally, it is demonstrated that highly anisotropic powders can also be obtained by dynamic-HDDR processing of stoichiometric Nd₂Fe₁₄B powders.     

Simultaneous enhancement in coercivity and remanence of Nd2Fe14B permanent magnet by grain boundary diffusion process using NdHx

We have successfully developed a Dy-free grain boundary diffusion process with neodymium hydride (NdH_x) alloy to the permanent magnet Nd₂Fe₁₄B powders using hydrogenation – disproportionation – desorption – recombination (HDDR) method. All the diffusion treatments were performed at 700–800 °C for various annealing time under the high vacuum with rotating diffusion method that effectively control the abnormal grain growth. The coercivities of Dy-treated Nd₂Fe₁₄B powders were varied from 9.5 kOe to 13.2 kOe but the remanence was decreased to 8.1 kG (10% reduction) depending on dysprosium hydride (DyH_x) content and diffusion treated time. However, the coercivity and remanence of Dy-free diffusion treated powder have been increased to 12.2 kOe (28.5% enhancement) and 11.1 kG (22% enhancement) at the optimal diffusion treatment (800 °C for 3 h), respectively. This unique simultaneous enhancement is to isolate the magnetic coupling between Nd₂Fe₁₄B grains by creating non-magnetic Nd grain boundaries and enhance the alignment of the Nd₂Fe₁4B hard magnetic phase, fabricated by optimal diffusion conditions.     

Preparation,microstructure, and magnetic properties of a nanocrystalline Nd12Fe82B6 alloy by HDDR combined with mechanical milling

Nanocrystalline Nd₁₂Fe₈₂B₆ (atomic ratio) alloy powders with Nd₂Fe₁₄B/α-Fe two-phase structure were prepared by HDDR combined with mechanical milling. The as-cast Nd₁₂Fe₈₂B₆ alloy was disproportionated via ball milling in hydrogen, and desorption–recombination was then performed. The phase and structural change due to both the milling in hydrogen and the subsequent desorption–recombination treatment was characterized by X-ray diffraction (XRD). The desorption–recombination behavior of the as-disproportionated alloy was investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The morphology and microstructure of the final alloy powders subject to desorption–recombination treatment were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results showed that, by milling in hydrogen for 20 h, the matrix Nd₂Fe₁₄B phase of the alloy was fully disproportionated into a nano-structured mixture of Nd₂H₅, Fe₂B, and α-Fe phases with average size of about 8 nm, and that a subsequent desorption–recombination treatment at 760 °C for 30 min led to the formation of Nd₂Fe₁₄B/α-Fe two-phase nanocomposite powders with average crystallite size of 30 nm. The remanence B_r, coercivity H_c, and maximum energy product (BH)_max of such nanocrystalline Nd₁₂Fe₈₂B₆ alloy powders achieved 0.73 T, 610 kA/m, and 110.8 kJ/m³, respectively.     

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.     

NdFeB纳米复合永磁材料的交换耦合相互作用和有效各向异性

以Nd₂Fe₁₄B/αFe为例，采用立方体晶粒结构模型，研究了纳米复合永磁材料中不同磁性晶粒间的交换耦合相互作用和有效各向异性.纳米复合永磁材料的有效各向异性Keff等于软、硬磁性相各向异性的统计平均值，每个晶粒的各向异性由晶粒表面交换耦合部分和晶粒内部未交换耦合部分的各向异性共同确定.计算结果表明，软、硬磁性相晶粒尺寸分布显著地影响有效各向异性Keff的值.当软、硬磁性晶粒尺寸D相同时，Keff随晶粒尺寸和硬磁性相体积分数的降低而减小, 当D<20nm 时，K 关键词： 纳米复合永磁材料 交换耦合相互作用 有效各向异性 晶粒尺寸     

Preparation and Properties of Iron and Iron Oxide Nanocrystals in MgO Matrix

We have prepared α-iron and magnetite (Fe₃O₄) nanoparticles in MgO matrix from a mixture of nanocrystalline Fe₂O₃ with Mg(H,O) powders calcinated in hydrogen. This procedure yielded spherical magnetic nanoparticles embedded in MgO. Transmission electron microscopy and Mössbauer spectroscopy were used for structure and phase analysis. The measurements of magnetic properties showed increased coercivity of the nanocomposite samples.     

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.     

Investigation on magnetic properties of orientated nanocomposite Pr2Fe14B/α-Fe permanent magnets by micromagnetic finite-element method

Demagnetization curves for nanocomposite Pr₂Fe₁₄B/α-Fe permanent magnets with different hard grain alignment are calculated by a micromagnetic finite-element method. The results show that both remanence and coercivity increase with improving hard grains alignment. The demagnetization curves show a single-phase demagnetization behavior for the samples with grain size d of 10 nm and two-phase behavior for the samples with d of 20 and 30 nm. H_ex (reflecting the magnetic hardening of α-Fe) and H_irr (expressing the irreversible reversal of hard phase) are both enhanced with improving the hard grain alignment. The magnetic reversal in orientated nanocomposite permanent magnets is mainly controlled by inhomogeneous pinning of the nucleated type.     

Synthesis, structural and magnetic properties of the nanocomposite Fe63B23Nd7Y3Nb3Cr1 magnets

The Fe₆₃B₂₃Nd₇Y₃Nb₃Cr₁ nanocomposite magnets in the form of sheets have been prepared by copper mold casting technique. The phase evolution, crystal structure, microstructural and magnetic properties have been investigated in the as-cast and annealed states. The as-cast sheets show magnetically soft behaviors which become magnetically hard by thermal annealing. The optimal annealed microstructure was composed of nanosize soft magnetic α-Fe (19-29 nm) and hard magnetic Nd₂Fe₁₄B (45-55 nm) grains. The best hard magnetic properties such as intrinsic coercivity, _jH_c of 1119 kA/m, remanence, B_r of 0.44 T, magnetic induction to saturation magnetization ratio, M_r/M_s=0.61 and maximum energy product, (BH)_max of 55 kJ/m³ was obtained after annealing at 680 °C for 15 min. The annealing treatment above 680 °C results in non-ideal phase grains growth, which degrade the magnetic properties.     

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.     

Refinement of the microstructure and enhancement of the magnetic properties in α-Fe/(Nd,Dy)2Fe14B nanocomposite using the two-step annealing technique

The Nd_8−xDy_xFe_87.5B_4.5 (x=0–1.0$x=0–1.0$) nanocomposites have been prepared by melt spinning and subsequent two-step heat treatment technique. The crystallization behaviors, microstructures and magnetic properties of the samples have been investigated. The experimental results show that the crystallization temperature of α-Fe soft phase has no obvious change through Dy addition while the crystallization temperature of 2:14:1 hard phase increases remarkably with increasing Dy content. By adopting a two-step heat treatment technique, a finer and more uniform microstructure can be developed. A dramatic enhancement of remanence J_r from 0.84 to 1.1 T, coercivity H_cj from 417 to 520 kA/m and energy product (BH)_m from 76.8 to 110 kJ/m³ have been obtained in Nd₇Dy₁Fe_87.5B_4.5 (30 vol%α-Fe ) nanocomposite.     

Angular dependence of the coercive force of textured rare earth permanent magnets

On the basis of model calculations experimental results on the angular dependence of the coercivity H_c and the remanence coercivity H_R of hard magnetic materials of the type SmCo₅, Sm₂(Co, Fe, Cu, Zr)₁₅ and Nd₂Fe₁₄B are discussed. In the model coherent rotation as well as incoherent magnetization jumps (e.g. 180°-Bloch walls) are included. The texture is described by an axial symmetric distribution of the easy axes with only oneparameter. For Sm₂(Co, Fe, Cu, Zr)₁₅ the model explains irreversible (H_R (θ)-curves) as well as reversible (H_R(θ)−H_c(θ)) magnetization processesin good agreement with the experiments, whereas stronger deviations exist for SmCo₅ and Nd₂Fe₁₄B, especially in the H_c(θ)-curves. These deviations should be caused by other reversible magnetization processes     

Nd-Fe(Co,Nb)-B交换耦合磁体的磁性

用熔体快淬法结合热处理制备了高性能纳米复合永磁合金Nd₉Fe_85.5-xCo_xNb₁B_4.5(0≤x≤16).最佳磁性能对应的成分为Nd₉Fe_81.5Nb₁B_4.5,其永磁性能如下：最大磁能积(BH)_max＝156kJ/m³,剩磁J_r＝1.11T 关键词：