Effect of element substitution on nanostructure and hard magnetism of rapidly quenched Nd2Fe14B

The structural and magnetic properties of Nd₁₂Fe₈₂B₆ and Nd₁₀M₂Fe₈₂B₆ (M = Nb, Ti, Zr, Cr) alloys prepared using arc melting and melt spinning have been investigated. All the samples are found to crystallise with a tetragonal Nd₂Fe₁₄B phase without any alloy or elemental impurities. There is a small decrease in the unit cell volume of Nd₂Fe₁₄B due to transition metal (M) addition. The substitution of Nb and Ti refines and homogenises the nanostructure of the alloys, promoting intergrain exchange coupling leading to an increase in the remanence and energy product. For example, the remanence and energy product of Nd₁₂Fe₈₂B₆ and Nd₁₀Nb₂Fe₈₂B₆ are 8.4 kG and 15 MGOe, and 9.9 kG and 20 MGOe, respectively. The J(T) curves are similar to those of a single phase ferromagnetic material suggesting no segregation of ferromagnetic impurities. The observed structural and magnetic properties are consistent with the fact that the substitutional transition metal atoms occupy the Nd site of the tetragonal Nd₂Fe₁₄B crystal lattice. The improvement of magnetic properties of nanocrystalline Nd₂Fe₁₄B alloys with the decrease in Nd concentration may be beneficial for the application of this material in bonded magnets.     

Phase formation in undercooled NdFeB alloy droplets

Small droplets of Nd_xFe_100−1.5xB_0.5x alloys (x=11.8–15) were undercooled and solidified using the drop tube technique for the purpose of studying metastable phase formation in this technically important alloy system. It was found that primary γ-Fe phase has been suppressed in most of the droplets due to significant undercooling levels achieved prior to solidification. Consequently, the primary crystallization either of metastable Nd₂Fe₁₇B_y (y≈1) phase or of Nd₂Fe₁₄B phase has been favored. The former occurs predominantly to low Nd alloys (x=11.8–13), while the latter prevails in Nd-rich alloys (x=14–15). By means of thermomagnetic analysis and powder X-ray diffraction analysis, it was determined that the metastable Nd₂Fe₁₇B_y phase has a Curie temperature of about 100°C and a hexagonal structure with lattice parameters as a=0.496 and c=0.416 nm.     

(Nd1－xGdx)3Fe27.31Ti1.69化合物的结构和磁性

通过X射线衍射和磁性测量等手段研究了(Nd_1-xGd_x)₃Fe_27.31Ti_1.69(0≤x≤0.6)化合物的结构和磁性.X射线衍射测量结果表明Gd替代后并未改变Nd₃(Fe,Ti)₂₉化合物的晶体结构，但引起了晶胞体积收缩.随着Gd含量的增加，化合物的居里温度T_C和室温磁晶各向异性场B_a单调增加，而自旋重取向 关键词： 1-xGd_x)₃Fe_27.31Ti_1.69化合物')" href="#">(Nd_1-xGd_x)₃Fe_27.31Ti_1.69化合物 磁晶各向异性 自旋重取向 磁相图     

Dendrite growth characteristics within liquid Fe-Sb alloy

Bulk samples and small droplets of liquid Fe-10%Sb alloys are undercooled up to 429 K (0.24TL) and 568 K (0.32TL), respectively, with glass fluxing and free fall techniques. The high undercooling does not change the phase constitution, and only the αFe solid solution is found in the rapidly solidified alloy. The experimental results show that when the undercooling is below 296 K, the growth velocity of αFe dendrite rises exponentially with the increase of undercooling and reaches a maximum value 1.38 m/s. S...     

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.     

Solidification mechanism transition of liquid Co–Cu–Ni ternary alloy

We report a solidification mechanism transition of liquid ternary Co₄₅Cu₄₅Ni₁₀ alloy when it solidifies at a critical undercooling of about 344 K. When undercooling at ΔT<344 K, the solidification process is characterized by primary S (Co) dendritic growth and a subsequent peritectic transition. The dendritic growth velocity of S (Co) dendrite increases with the rise of undercooling. However, once ΔT>344 K, the solidification velocity decreases with the increase of undercooling. In this case, liquid/liquid phase separation takes place prior to solidification. The minor L₂ (Cu) droplets hinder the motion of the solidification front, and a monotectic transition may occur in the major L₁ phase. These facts caused by metastable phase separation are responsible for the slow growth at high undercoolings.     

Glass-forming ability and thermal stability of Fe<Subscript>62</Subscript>Nb<Subscript>8−x</Subscript>Zr<Subscript>x</Subscript>B<Subscript>30</Subscript> and Fe<Subscript>72</Subscript>Zr<Subscript>8</Subscript>B<Subscript>20</Subscript> amorphous alloys?

Glass-forming ability (GFA) and thermal stability of Fe₆₂Nb₈B₃₀, Fe₆₂Nb₆Zr₂B₃₀ and Fe₇₂Zr₈B₂₀ at % amorphous alloys were investigated by calorimetric (DSC and DTA) measurements. The crystallization kinetics was studied by DSC in the mode of continuous versus linear heating and it was found that both the glass transition temperature, T _g , and the crystallization peak temperature, T _p , display strong dependence on the heating rate. The partial replacement of Nb by Zr leads to lower T _g and T _x temperatures and causes a decrease of the supercooled liquid region. JMA analysis of isothermal transformation data measured between T _g and T _x suggests that the crystallization of the Fe₆₂Nb₈B₃₀ and Fe₆₂Nb₆Zr₂B₃₀ amorphous alloys take place by three-dimensional growth with constant nucleation rate. Nb enhances the precipitation of the metastable Fe₂₃B₆ phase and stabilizes it up to the third crystallization stage. Zr addition increases the lattice constant of Fe₂₃B₆ and, at the same time, decreases the grain size.     

热处理对非晶态合金Nd4Fe96-xBx磁性的影响

本文研究了用单辊急冷方法制备的非晶态合金Nd₄Fe_96-xB_x的晶化,以及热处理对其硬磁性和相组成的影响,发现非晶态合金Nd₄Fe_96-xB_x的晶化温度比相同B含量的非晶态合金Fe_100-xB_x高120—190K,X射线衍射和热磁测量表明,15≤x≤25的样品晶化相是由Nd₂Fe₁₄B(T 关键词：     

Microstructure evolution of undercooled Fe-Co-Cu alloys

Rapid solidification of undercooled Fe-Co-Cu alloys was investigated by means of fluxing purification and cyclic superheating technique. A transition in microstructure from dendrites to phase-separation occurred above a phase-separation undercooling ΔT_sep. When ΔT<ΔT_sep, dendrite was observed, the trunks were rich in Fe and Co, while Cu was rich at inter-dendrites. However, the phase-separated microstructure was obtained once ΔT>ΔT_sep, with a large sphere of L1 phase located almost at the center of the sample and enwrapped by L2 phase. ΔT_sep was 222, 88 and 45 K for Fe₅₀Co₃₀Cu₂₀, Fe₂₅Co₂₅Cu₅₀ and Fe₁₅Co₁₅Cu₇₀ alloys in this work, respectively. It was investigated that L1 phase solidified before L2 phase after liquid separation and followed different ways.     

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.     

Critical phenomena of amorphous Nd4(Fe0.75Cr0.25)77.5B18.5 alloys

The magnetic behavior of amorphous Nd₄(Fe_0.75Cr_0.25)_77.5B_18.5 alloys was investigated in the critical region. The Curie temperature T_C and critical exponents β, γ and δ are found to be 141 K, 0.45±0.02, 1.64±0.08 and 4.66±0.10, respectively. The data are fitted to a magnetic equation of state characteristic of a second-order phase transition over a rather wide range of temperatures both above and below T_C. It is noted that the values of the exponents are in disagreement with those derived for a three-dimensional Heisenberg ferromagnet and show an enhancement. This anomalous critical behavior may originate from magnetic inhomogeneity.     

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.     

Mössbauer Study of the Fe3B/Nd2Fe14B Nanocomposite Magnet by the Addition of Co

The addition of Co to Nd₄Fe_77.5–x Co _x Hf_0.5Ga_0.5B_18.5 (0x5) was found to enhance the magnetic properties of Fe₃B/Nd₂Fe₁₄B nanocomposite magnets. The enhancement resulted from the fact that Co tends to retard the formation of Fe₃B from the amorphous matrix but to accelerate that of Nd₂Fe₁₄B. The decreased interval between the crystallization temperature of Fe₃B and Nd₂Fe₁₄B led to a uniform grain size distribution of both phases during the annealing treatment. The additive Co was confirmed to partition mainly to Nd₂Fe₁₄B crystals rather than to Fe₃B which was traced by XRD and Mössbauer spectroscopy as well. About 72 vol.% of Fe₃B, 27 vol.% of Nd₂Fe₁₄B, and a small amount of Fe around 1 vol.%, respectively, were found to form. However, the volume fraction of each phase did not vary by the addition of Co up to 5 at.%.     

Magnetic properties of the Nd<Subscript>0.5</Subscript>Gd<Subscript>0.5</Subscript>Fe<Subscript>3</Subscript>(BO<Subscript>3</Subscript>)<Subscript>4</Subscript> single crystal

The magnetic properties of the Nd_0.5Gd_0.5Fe₃(BO₃)₄ single crystal have been studied in principal crystallographic directions in magnetic fields to 90 kG in the temperature range 2–300 K; in addition, the heat capacity has been measured in the range 2–300 K. It has been found that, below the Néel temperature T _N = 32 K down to 2 K, the single crystal exhibits an easy-plane antiferromagnetic structure. A hysteresis has been detected during magnetization of the crystal in the easy plane in fields of 1.0–3.5 kG, and a singularity has been found in the temperature dependence of the magnetic susceptibility in the easy plane at a temperature of 11 K in fields B < 1 kG. It has been shown that the singularity is due to appearance of the hysteresis. The origin of the magnetic properties of the crystal near the hysteresis has been discussed.     

Nd composition dependence of microstructure and magnetic properties for gradient sputtered NdFeB films

NdFeB films with Nd compositions varied from 13.34 to 24.30 at% were deposited by DC gradient sputtering using targets Nd_12.5Fe_71.5B₁₆ and Nd. The hard magnetic properties, grain growth direction and magnetic domain structures were dramatically influenced by Nd composition. The samples with intermediate Nd concentrations exhibited optimal magnetic properties and microstructures, such as large squareness ratio over 0.9, large energy product up to 174 kJ/m³, and vertical domain structure. However, the samples with higher and lower Nd compositions showed almost isotropic loops. (0 0 l) as main X-ray diffraction peaks in the optimal Nd composition region indicated most of Nd₂Fe₁₄B grains with c-axis perpendicular to the film plane, while NdFeB grains in other region are almost random growth. The good magnetic properties can be attributed to the vertical growth of Nd₂Fe₁₄B grains.     

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.     

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 Mössbauer study of Nd−Fe−Co−B permanent magnetic alloys

Sintered Nd₁₇ (Fe_1?x Co_x)₇₅B₈ permanent magnetic alloys have been studied by Mössbauer effect, X-ray diffraction and electron probe micro-analysis, The results show that the alloys are composed of the tetragonal phase Nd₂(Fe,Co)₁₄B, the B-rich phase Nd₁₁₁(Fe,Co)₄B₄ and the Nd-rich phase Nd₈₀(Fe,Co)₁₉B. In the tetragonal phase, Co atoms occupy preferentially the k₂ and j₂ sites, and Fe atoms occupy randomly the k₁ site and preferentially the j₁ site while the e and c sites seem to be completely occupied by Fe atoms.     

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.     

Die-upset Nd11.5Fe72.4Co9Nb1B6.1 magnets with additions of Zn, Al and Sn

The magnetic properties and microstructure were studied for bulk Nd_11.5Fe_72.4Co₉Nb₁B_6.1 magnets synthesized by hot-pressing and subsequent die-upsetting the melt-spun ribbons with additions of three kinds of low-melting-point metal (Zn, Al and Sn). Die-upset Nd_11.5Fe_72.4Co₉Nb₁B_6.1 magnets have low magnetic properties since they have an inhomogeneous microstructure with many coarse grains. The microstructure of die-upset magnets remains almost unchanged with Al and Sn additions, which only have negative effects on the magnetic properties. Different from Al and Sn additions, Zn addition changes the phase composition of the starting melt-spun powers due to the reaction of Zn and Nd₂Fe₁₄B during hot-pressing and hot-deforming and enhances the development of the desired [0 0 1] texture and improves the microstructure of die-upset magnets. As a result, an anisotropic magnet with good maximum energy product (221 kJ/m³) and high coercivity (670 kA/m) is obtained by adding 2 wt% Zn to the Nd_11.5Fe_72.4Co₉Nb₁B_6.1 alloy.