Toward understanding the microstructure characteristics,phase selection and magnetic properties of laser additive manufactured Nd-Fe-B permanent magnets

Nd-Fe-B permanent magnets play a crucial role in energy conversion and electronic devices.The essential magnetic properties of Nd-Fe-B magnets,particularly coercivity and remanent magnetization,are significantly infuenced by the phase characteristics and microstructure.In this work,Nd-Fe-B magnets were manufactured using vacuum induction melting(VIM),laser directed energy deposition(LDED)and laser powder bed fusion(LPBF)technologies.Themicrostructure evolution and phase selection of Nd-Fe-B magnets were then clarified in detail.The results indicated that the solidification velocity(V)and cooling rate(R)are key factors in the phase selection.In terms of the VIM-casting Nd-Fe-B magnet,a large volume fraction of theα-Fe soft magnetic phase(39.7 vol.%)and Nd2Fe17Bxmetastable phase(34.7 vol.%)areformed due to the low R(2.3×10-1?C s-1),whereas only a minor fraction of the Nd2Fe14B hard magnetic phase(5.15 vol.%)is presented.For the LDED-processed Nd-Fe-B deposit,although the Nd2Fe14B hard magnetic phase also had a low value(3.4 vol.%)as the values of V(<10-2m s-1)and R(5.06×103?C s-1)increased,part of theα-Fe soft magnetic phase(31.7vol.%)is suppressed,and a higher volume of Nd2Fe17Bxmetastable phases(47.5 vol.%)areformed.As a result,both the VIM-casting and LDED-processed Nd-Fe-B deposits exhibited poor magnetic properties.In contrast,employing the high values of V(>10-2m s-1)and R(1.45×106?C s-1)in the LPBF process resulted in the substantial formation of the Nd2Fe14B hard magnetic phase(55.8 vol.%)directly from the liquid,while theα-Fe soft magnetic phase and Nd2Fe17Bxmetastable phase precipitation are suppressed in the LPBF-processed Nd-Fe-B magnet.Additionally,crystallographic texture analysis reveals that the LPBF-processedNd-Fe-B magnets exhibit isotropic magnetic characteristics.Consequently,the LPBF-processed Nd-Fe-B deposit,exhibiting a coercivity of 656 k A m-1,remanence of 0.79 T and maximum energy product of 71.5 k J m-3,achieved an acceptable magnetic performance,comparable to other additive manufacturing processed Nd-Fe-B magnets from MQP(Nd-lean)Nd-Fe-Bpowder.

Effect of TbF_(3)diffusion on the demagnetization behavior and domain evolution of sintered Nd-Fe-B magnets by electrophoretic deposition

We studied the magnetic properties and domain evolution of annealed and TbF3-diffused sintered Nd-Fe-B magnets using the electrophoretic deposition method.After TbF_(3)diffusion,the coercivity increased significantly by 9.9 kOe and microstructural analysis suggested that Tb favored the formation of the(Nd,Tb)_(2)Fe_(14)B shell phase in the outer region of the matrix grains.The first magnetization reversal and the dynamic successive domain propagation process were detected with a magneto-optical Kerr microscope.For the TbF_(3)-diffused magnet,the magnetization reversal appeared at a larger applied field and the degree of simultaneous magnetization reversal decreased compared with an annealed magnet.During demagnetization after full magnetization,the occurrence of domain wall motion(DWM)in the reproduced multi-domain regions was observed by the step method.The maximum polarization change resulting from the reproduced DWM was inversely related to the coercivity.The increased coercivity for the diffused magnet was mainly attributed to the more difficult nucleation of the magnetic reversed region owing to the improved magneto-crystalline anisotropy field as a result of Tb diffusion.

Microstructure and magnetic properties of anisotropic Nd-Fe-B magnets prepared by spark plasma sintering and hot deformation

Bulk anisotropic Nd-Fe-B magnets were prepared from hydrogen-disproportionation-desorption-recombination（HDDR） powders via spark plasma sintering（SPS） and subsequent hot deformation. The influence of sintering temperature on the structure and magnetic properties of the spark plasma sintered Nd-Fe-B magnets were studied. The remanence Br, intrinsic coercivity Hcj, and the maximum energy product（BH）max, of sintered Nd-Fe-B magnets first increase and then decrease with the increase of sintering temperature, TSPS, from 650 °C to 900 °C. The optimal magnetic properties can be obtained when TSPS is 800 °C. The Nd-Fe-B magnet sinter treated at 800 °C was subjected to further hot deformation. Compared with the starting HDDR powders or the SPS treated magnets, the hot-deformed magnets present more obvious anisotropy and possess much better magnetic properties due to the good c-axis texture formed in the deformation process. The anisotropic magnet deformed at 800 °C with 50% compression ratio has a microstructure consisting of well aligned and platelet-shaped Nd2Fe14 B grains without abnormal grain growth and exhibits excellent magnetic properties parallel to the pressing axis.

Magnetic microstructure and coercivity mechanism of high performance Nd-Fe-B magnets

Magnetic microstructure of high performance Nd-Fe-B magnets was investigated by using magnetic force microscopy. The correlation between magnetic microstructure and coercivity for high performance Nd-Fe-B magnets was studied. It is found that the magnets with different coercivity mechanism take on different microstructures and magnetism. Moreover, the magnetic microstructures of high performance permanent magnets can be explained by the starting field theory model.

Electrochemical Corrosion Behavior of Nd-Fe-B Sintered Magnets in Different Acid Solutions

Electrochemical corrosion behavior of Nd-Fe-B sintered magnets in nitric acid, hydrochloric acid, sulfuric acid, phosphate acid and in oxalic acid was studied. Potentiodynamic polarization curves and immersion time dependence of corrosion rates of Nd-Fe-B sintered magnets in different acid solutions were tested. Microstructures of corroded Nd-Fe-B sintered magnets were investigated by means of SEM and AFM. The results indicate that in strong acid solutions of similar hydrogen ion concentration, the corrosion current increases in the order of HCl 〉 H3SO4 〉 HNO3 solution and Nd-Fe-B sintered magnets are passivated in phosphate acid and oxalic acid. Within 25 min, the corrosion rates of Nd-Fe-B sintered magnets in H2SO4 and H3PO4 solutions show a declining trend with immersion time, while in HNO3 and HCl solutions the corrosion rates are rising. And in H2C2O4 solution, weight of the magnets increases. The brim of Nd-Fe-B sintered magnets is corroded rather seriously and the size of the magnets changed greatly in nitric acid. The surfaces of the corroded magnets in the above mentioned acid solutions are all coarse.

Grain Growth Behavior in Sintered Nd-Fe-B Magnets

The Nd2Fe14B grain growth behavior in sintered Nd-Fe-B magnets was quantitatively described.The effects of sintering temperature and time,and alloy powder size and its distribution on grain growth process were analyzed.Hence,possible grain growth mechanisms in these magnets were qualitatively discussed.The Nd2Fe14B grain growth proceeded at quite a high rate in the initial 0~1 h of sintering and from then onwards the grain growth rate decreased.A large average particle size or a wide particle size distribution of initial alloy powders was found to remarkably accelerate the grain growth process and even result in the occurrence of abnormal grain growth.On the basis of experimental results,two grain growth mechanisms were considered to operate during sintering of Nd-Fe-B magnets,that is,dissolution and re-precipitation of Nd2Fe14B particles,and Nd2Fe14B particle growth by coalescence.It was believed that Nd2Fe14B particle growth by coalescence not only produced a large average grain size and a wide grain size distribution,but also was the fundamental reason for the formation of abnormally large grains in the microstructure of sintered Nd-Fe-B magnets.

Effect of bonding process on the properties of isotropic epoxy resin-bonded Nd-Fe-B magnets

Bonded NdFeB magnets were prepared by compression molding. The effect of preparation technology on their magnetic and mechanical properties was studied through the analysis of density, Br, Hcj, （BH）max, bending strength, and compressive strength of the bonded magnets. The results showed that the magnetic properties decreased with increasing binder content, whereas the mechanical properties increased. Br and （BH）max increased with rising pressure, whereas Hcj decreased. For a fixed mass fraction of the binder, the optimal pressure was 620 MPa and the best thermosetting temperature was 160°C. These conditions made the bonded magnets have the optimal mechanical properties. Scanning electron microscopy （SEM） analyses of the fracture surfaces indicated that the epoxy resin bonded magnets exhibited brittle behavior.

Magnetoresistive behavior and magnetization reversal of NiFe/Cu/CoFe/IrMn spin valve GMRs in nanoscale

The magnetoresistance behavior and the magnetization reversal mode of NiFe/Cu/CoFe/IrMn spin valve giant magnetoresistance （SV-GMR） in nanoscale were investigated experimentally and theoretically by nanosized magnetic simulation methods. Based on the Landau-Lifshitz-Gilbert equation, a model with a special gridding was proposed to calculate the giant magnetoresistance ratio （MR） and investigate the magnetization reversal mode. The relationship between MR and the external magnetic field was obtained and analyzed. Studies into the variation of the magnetization distribution reveal that the magnetization reversal mode, that is, the jump variation mode for NiFe/Cu/CoFe/IrMn, depends greatly on the antiferromagnetic coupling behavior between the pinned layer and the antiferromagnetic layer. It is also found that the switching field is almost linear with the exchange coefficient.

Thermal Stability of Low Cost Nd-Fe-B Magnets

1.IntroductionSince the Nd-Fe-B magnets appearedin 1983,researchers,producers and users ofthe permanent magnetic materials have paidgreat attention to them.Because the mag-nets have low Curie temperature Tc andbad thermal stability as well as easeoxidation,their applications are limited insome fields.The researchers are greatly in-terested in increase energy product

Magnetic properties and thermal stability of anisotropic bonded Nd-Fe-B magnets by warm compaction

Anisotropic bonded magnets were prepared by warm compaction using anisotropic Nd-Fe-B powder. The forming process, magnetic properties, and temperature stability were studied. The results indicate that the optimal temperature of the process, which was decided by the vis-cosity of the binders, was 110°C. With increasing pressure, the density of the magnets increased. When the pressure was above 700 MPa, the powder particles were destroyed and the magnetic properties decreased. The magnetic properties of the anisotropic bonded magnets were as follows： remanence Br=0.98 T, intrinsic coercivity iHc=1361 kA/m, and maximum energy product BHmax=166 kJ/m3. The magnets had excellent thermal stability because of the high coercivity and good squareness of demagnetization curves. The flux density of the magnets was 35% higher than that of isotropic bonded Nd-Fe-B magnets at 120°C for 1000 h. The flux density of the bonded magnets showed little change with regard to temperature.

Temperature stability and microstructure of ultra-high intrinsic coercivity Nd-Fe-B magnets

The variations of intrinsic coercivity and remanence of sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity were investigated. The results showed that the intrinsic coercivity and remanence declined simultaneously with increasing temperature, but the squareness of the magnets has hardly been changed. The temperature coefficients of remanence （α） and coercivity （β） for the magnets were calculated by two different methods, and the variations of the temperature coefficients and the microstructure of sintered Nd-Fe-B magnets were analyzed. The temperature coefficients of remanence （α） and coercivity （β） for the sintered magnets are very small, and the existence of fine microstructure is necessary to obtain sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity.

Research of warm compaction technology on nylon bonded Nd-Fe-B magnets

Warm compaction and room temperature compaction were applied to prepare bonded Nd-Fe-B magnets. The results indicated that the density of magnet was determined by the compaction pressure and warm compaction temperature, whereas, the thermosetting temperature could hardly affect the density of magnet. The mechanical properties of magnets were the best when the thermosetting temperature was 200 ℃. The Br, Hob, and （BH）max of warm compaction magnet were higher than those of room compaction. When the warm compaction temperature and thermosetting temperature were invariable, the density of magnet increased with the increase of compaction pressure, which resulted in the increase of Br, Hcb, and （BH）max of magnet and the decrease of Hcj of magnet. When the warm compaction temperature and compaction pressure were invariable, the magnetic properties of magnets decreased with the increase of thermosetting temperature. The magnetic properties of warm compaction molding magnets were better than those of injection molding magnets.

An Efficient Process for Recycling Nd-Fe-B Sludge as High-Performance Sintered Magnets

Given the increasing concern regarding the global decline in rare earth reserves and the environmental burden from current wet-process recycling techniques,it is urgent to develop an efficient recycling technique for leftover sludge from the manufacturing process of neodymium-iron-boron(Nd-Fe-B)sintered magnets.In the present study,centerless grinding sludge from the Nd-Fe-B sintered magnet machining process was selected as the starting material.The sludge was subjected to a reduction-diffusion(RD)process in order to synthesize recycled neodymium magnet(Nd2Fe14B)powder;during this process,most of the valuable elements,including neodymium(Nd),praseodymium(Pr),gadolinium(Gd),dysprosium(Dy),holmium(Ho),and cobalt(Co),were recovered simultaneously.Calcium chloride(CaCl2)powder with a lower melting point was introduced into the RD process to reduce recycling cost and improve recycling efficiency.The mechanism of the reactions was investigated systematically by adjusting the reaction temperature and calcium/sludge weight ratio.It was found that single-phase Nd2Fe14B particles with good crystallinity were obtained when the calcium weight ratio(calcium/sludge)and reaction temperature were 40 wt% and 1050℃,respectively.The recovered Nd2Fe14B particles were blended with 37.7 wt% Nd4Fe14B powder to fabricate Nd-Fe-B sintered magnets with a remanence of 12.1 kG(1 G=1×10^-4T),and a coercivity of 14.6 kOe(1 Oe=79.6A·m^-1),resulting in an energy product of 34.5 MGOe.This recycling route promises a great advantage in recycling efficiency as well as in cost.

Effect of optimal aging treatment on magnetic performance and mechanical properties of sintered Nd-Fe-B permanent magnets

The magnetic performance and mechanical properties including hardness, brittleness, fracture toughness and strength characteristics of the as-sintered and the optimal aged Nd-Fe-B magnets were examined in this work. A new method of Vickers hardness indentation combined with acoustic emission was used to test the brittleness of the magnets.The results show that the magnetic properties of the magnets could be improved through aging treatment, especially the intrinsic coercive force. But it is accompanied by a decrease of strength and fracture toughness. Theoretical calculation confirms that acoustic emission energy accumulated count value could be used to characterize the material brittleness. The bending fracture morphologies of the as-sintered and the optimal aged Nd Fe B magnets were investigated with the emphasis on the relationship between mechanical properties and microstructure using a field emission scanning electron microscopy(FE-SEM). The research results indicate that the intergranular fracture is the primary fracture mechanism for both as-sintered and optimal aged Nd Fe B magnets. Aging treatment changes the morphology and distribution of the Nd-rich phases, reducing the sliding resistance between Nd_2Fe_(14)B main crystal grains and lowers the grain boundary strength, which is the main reason for the strength and fracture toughness decrease of the aged Nd-Fe-B magnets.

Structure and Magnetic Properties of Fe_(76.5)Si_(13.5)B_9Cu_1 Alloy with Nanoscale Grain Size

The structure and magnetic properties of Fe76.5Si13.5B9Cu1 alloys with a nanocrystalline (NC) bcc Fe(Si) phase trom about 23 to 46 nm in diameter, which were first formed into amorphous ribbons and then annealed at various temperatures between 703 and 773 K, have been investigated. At annealing temperatures from 703 to 748 K, the single NC bcc(Si) phase is obtained in the crystallized alloys. The grain size and the Si-content in the NC bcc Fe(Si) phase for the alloys annealed at different temperatures are presented. The soft magnetic properties and the saturation magnetostriction for the alloys with the NC bcc Fe(Si) phase are also measured. The results show that, the saturation magnetizotion and the permeability are improved for the alloys with only the NC bcc Fe(Si) phase and become better with decreasing of the NC bcc phase size, and the saturation magnetostriction declines for the alloys with increasing Si-content in the NC bcc Fe(Si) phase.

Reduction of Sensitivity to Sintering Temperature for Nd-Fe-B Magnets through Zr and Nb Additions

To reduce the sensitivity of grain growth to sintering temperature for improving property consistency of sintered Nd-Fe-B magnets, combined additions of Zr and Nb were investigated. It was found that when Zr content was increased to 0.07 at. pct, abnormal grain growth was effectively hindered even when the sintering temperature reached 1100℃. With combined additions of 0.07 at. pct Zr and 0.07 at. pct Nb, the sensitivity of grain growth to sintering temperature was greatly reduced consistency than the magnets containing no Zr and also improved. The magnets sintered at 1100℃ showed higher property Nb. In addition, the magnetic properties of magnets were also improved.

Statistical model of magnetization reversal in Nd-Fe-B sintered magnets

Statistical model of magnetization reversal was used to simulate the magnetization reversal behavior in the sintered Nd-Fe-B magnets with double grain-size distributions due to the abnormal grain growth (AGG). The magnetic properties and mechanical properties due to the formation of AGG grains in Nd-Fe-B sintered magnets were tested. The results show that the magnetic properties, especially the rectangularity were severely deteriorated after the formation of the AGG grains and a step was shown on the demagnetization curve, and the occurrence of AGG may account for the poor rectangularity and existence of the step on demagnetization curve according to the statistical model of magnetization reversal. The fracture toughness and bending strength are lowered because of the stress concentration in the AGG grains. The SEM images show that the formation of AGG grains is caused by the solid sintering due to the absence of RE-rich phase. Statistical model of magnetization reversal can qualitative by explain the dependence of the magnetization reversal behavior on the grain size in the Nd-Fe-B sintered magnets.

MAGNETIZATION BEHAVIOR IN SINTERED Nd-Fe-B MAGNETS

Magnetization and demagnetization curves and hysteresis loops applied different magnetizing.fields in sintered Nd-Fe-B and Nd-Dy-Fe-B magnets from thermally demagnetized and dc field-demagnetized states were investigated at temperatures of up to 150℃.The first-quadrant remagnetization curves and the curves of coercive forces _MH_C versus rernagnetizing fietds H_m from dc field-demagnetized state at room temperature show a step around magnetizing field as absolute value of the maximum intrinsic coercivity.The steps of _MH_C-H_m curves shifted to lower remagnetizing fields and the shapes of magnetization curves changed from step type to precipitous type when temperature went up to 100～150℃ or after the specimen was thermally demagnetized at a temperature higher than the Curie temperature.The steep rise of knee coereivity with increasing magnetizing field is behind that of _MH_C.Note that the magnetic hardening in sintered Nd-Fe-B magnets is controlled by pinning of domain walls.

Structure and Magnetic Properties of Nd-Fe-B/α-Fe Nanocomposite Magnets by Co, Nb, Dy Substitutions

Structure and magnetic properties of the nanocomposite magnets prepared by mechanical al loying procedure with composition 55 wt pct Nd (Fe0.92B0.08)5.5+45 wt pct α-Fe,55 wt pct Nd(Fe0.8-.Co0.12Nbx B0.08)5.5+45 wt pct α-Fe (x=0.00, 0.01- 0.03) and 55 wt pct (Nd0.9Dy0.1) (Fe0.77Co0.12Nb0.03B0.08)5.5+45 wt pct α-Fe were studied. It was found that substitution of Co for Fe could significantly improve the permanent magnetic properties of the nanocomposite magnets and typically, the maximum magnetic energy product was increased from 104.8 kJ/m3 (13.1 MGOe) to 141.6 kJ/m3 (17.7 MGOe). In contrast to the case of conventional nominally single-phase magnets, the addition of Nb results in promoting the growth of α-Fe grain and is thus unfavorable for the improvement of permanent magnetic properties of the nanocomposites. Although the addition of Dy can increase the coercivity of the magnets, the increase of magnetic anisotropy of hard phase leads to decrease of the critical grain size of soft phase. Additionally it causes the difficulty of preparing the nanocomposites because it is more difficult to control the grain size of soft phase to meet the requirement of appropriate exchange coupling between hard and soft grains

Temperature stability and fracture toughness of Nd-Fe-B magnets

Temperature stability and toughness of magnets are very important properties especially for application in motor. In this paper, it is found that temperature stability and toughness of magnets are improved when Fe is substituted with Co and heavy rare earth is substituted for Nd in part and suitable rich B grain-boundary phase is added. In addition, heavy rare earth substitution decreases the remanence temperature coefficient greatly, but has a little effect on Curie temperature of the magnets, which is beneficial to Nd-Fe-B magnets for the application in motor.