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.

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.

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.

Improvement in coercivity,thermal stability,and corrosion resistance of sintered Nd-Fe-B magnets with Dy_(80)Ga_(20) intergranular addition

To investigate the coercivity,corrosion resistance,and thermal stability of Nd-Fe-B magnets,their properties were investigated at room and high temperature before and after doping with Dy（80）Ga（20）（at.%） powder.The coercivity of the magnets increased from the undoped value of 12.72 kOe to a doped value of 21.44 kOe.A micro-structural analysis indicates that a well-developed core-shell structure forms in the magnets doped with Dy（80）Ga（20） powder.The improvement in magnetic properties is believed to be related to the refined and uniform matrix grains,continuous grain boundaries,and a hardened（Nd,Dy）2Fe（14）B shell surrounding the matrix grains.Additionally,the doped magnets exhibit an obvious improvement in thermal stability.For the magnets with added Dy（80）Ga（20） powder,the temperature coefficients of remanence（α） and coercivity（β） increased to-0.106%℃-（-1） and-0.60%℃-（-1） over the range 20-100 ℃,compared to temperature coefficients of-0.117%℃-（-1）（α） and-0.74%℃-（-1）（β） in the regular magnets without Dy（80）Ga（20） powder.The irreversible loss of magnetic flux（Hirr） was investigated at different temperatures.After being exposed to 150 ℃ for 2 h,the Hirr of magnets with 4 wt.%Dy（80）Ga（20） decreased by -95%compared to that of the undoped magnets.The enhanced temperature coefficients and Hirr indicate improved thermal stability in the doped Nd-Fe-B magnets.The intergranular addition of Dy（80）Ga（20） also improved the corrosion resistance of the magnets because of the enhanced intergranular phase.In a corrosive atmosphere for 96 h,the mass loss of the sintered magnets with 4 wt.%Dy（80）Ga（20） was 2.68 mg/cm-2,less than 10%of that suffered by the undoped magnets（28.1 mg/cm-2）.

Coercivity and microstructure of sintered Nd-Fe-B magnets diffused with Pr-Co,Pr-Al,and Pr-Co-Al alloys

The commercial 42 M Nd-Fe-B magnet was treated by grain boundary diffusion(GBD)with Pr_(70)Co_(30)(PC),Pr_(70)Al_(30)(PA)and Pr_(70)Co_(15)Al_(15)(PCA)alloys,respectively.The mechanism of coercivity enhancement in the GBD magnets was investigated.The coercivity was enhanced from 1.63 T to 2.15 T in the PCA GBD magnet,higher than the 1.81 T of the PC GBD magnet and the 2.01 T of the PA GBD magnet.This indicates that the joint addition of Co and Al in the diffusion source can further improve the coercivity.Microstructural investigations show that the coercivity enhancement is mainly attributed to the exchange-decoupling of the GB phases.In the PCA GBD magnet,the wider thin GB phases can be formed and the thin GB phases can still be observed at the diffusion depth of 1500μm due to the combined action of Co and Al.At the same time,the formation of the Pr-rich shell can also be observed,which is helpful for the coercivity enhancement.

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.

Investigation of Abnormal Grain Growth in Sintered Nd-Fe-B Permanent Magnet

The abnormal growth of grains of sintering Nd13.6 Dy0.4 Fe79.5 B6.5 magnets were investigated in low oxygen manufacturing process.The abnormal growth of grains occurs easily when the sintering temperature is higher than 1080℃ during the manufacture process.In the magnets, the oxygen content is less than 700 × 10-6 and the average particle size of powder is smaller than 4 μm.The squareness of demagnetization curve of magnet is deteriorated.For high performance magnets, the abnormal growth grain should be avoided by selecting a suitable sintering temperature.

Effect of annealing temperature on magnetic properties of a sintered Nd-Fe-B magnet after grain boundary diffusion with Dy_(70)Cu_(30) alloy

Grain boundary diffusion process(GBDP)has been developed as an effective approach to increase the coercivity of sintered Nd-Fe-B magnets by regulating the compositions and phase distributions near grain boundaries.This work aims to explore how to select the optimum annealing temperature after GBDP.In this work GBDP was performed on a sintered Nd-Fe-B magnet using Dy_(70)Cu_(30) alloy.After GBDP the low eutectic temperature of the grain boundary phases decreases from the initial 492 to 451℃.The magnetic property dependent on different annealing temperatures near the low eutectic temperature was studied.The magnetic properties,especially the squareness factor of demagnetization curve show a strong dependence on the annealing temperature.After GBDP the optimal magnetic properties can be obtained after annealing just above the low eutectic temperature of the grain boundary phases.The mechanism is discussed based on the microstructure analysis.

Optimization of core-shell structure distribution in sintered Nd-Fe-B magnets by titanium addition

In view of the uneven distribution of the core-shell structure of sintered Nd-Fe-B magnets after grain boundary diffusion,this study proposes to use high-melting-point and reactive element titanium(Ti)as an additive to increase the diffusion channels and to enhance the diffusion of heavy rare earth elements along the grain boundary phase.By adding Ti element,the diffusion depth and hence the intrinsic coercivity of magnets are increased significantly.The addition of Ti increases the coercivity at two stages:initially from 16.07 to 16.29 kOe by addition effect,and then from 16.29 to 25.16 kOe by facilitating the diffusion of Tb element.The formation of TiB_(2) phase improves the periodic arrangement of the crystal structure in the surroundings of the grain boundary phase and enhances its activity.The improved grain boundary diffusion and better core-shell structure distribution provide a theoretical guidance fo r solving the problem of diffusion depth in bulk magnets.

Effect of aluminum on microstructure and magnetic properties of sintered Nd-Fe-B magnets processed by grain boundary diffusion of Tb-Al

The grain boundary diffusion process(GBDP)of Tb can improve the coercivity of sintered Nd-Fe-B magnets.In this study,the effect of AI on the diffusion of Tb in the GBDP was investigated.The content of diffused Tb-Al was precisely controlled by adjusting the magnetron sputtering process.The Tb equivalent of Al was also studied.Results show that AI promotes the diffusion of Tb deeper into the magnet,reducing the thickness of the shell in the core-shell structure.This study is helpful for further developing the process,reducing the consumption of heavy rare earth elements(Tb),and improving the coercivity of sintered Nd-Fe-B magnets.

Impact Analysis of Microscopic Defect Types on the Macroscopic Crack Propagation in Sintered Silver Nanoparticles

Sintered silver nanoparticles(AgNPs)arewidely used in high-power electronics due to their exceptional properties.However,the material reliability is significantly affected by various microscopic defects.In this work,the three primary micro-defect types at potential stress concentrations in sintered AgNPs are identified,categorized,and quantified.Molecular dynamics(MD)simulations are employed to observe the failure evolution of different microscopic defects.The dominant mechanisms responsible for this evolution are dislocation nucleation and dislocation motion.At the same time,this paper clarifies the quantitative relationship between the tensile strain amount and the failure mechanism transitions of the three defect types by defining key strain points.The impact of defect types on the failure process is also discussed.Furthermore,traction-separation curves extracted from microscopic defect evolutions serve as a bridge to connect the macro-scale model.The validity of the crack propagation model is confirmed through tensile tests.Finally,we thoroughly analyze how micro-defect types influence macro-crack propagation and attempt to find supporting evidence from the MD model.Our findings provide a multi-perspective reference for the reliability analysis of sintered AgNPs.

Mechanical and corrosion properties of full liquid phase sintered WE43 magnesium alloy specimens fabricated via binder jetting additive manufacturing

This study investigates full liquid phase sintering as a process of fabrication parts from WE43(Mg-4wt.%Y-3wt.%RE-0.7wt.%Zr)alloy using binder jetting additive manufacturing(BJAM).This fabrication process is being developed for use in producing structural or biomedical devices.Specifically,this study focused on achieving a near-dense microstructure with WE43 Mg alloy while substantially reducing the duration of sintering post-processing after BJAM part rendering.The optimal process resulted in microstructure with 2.5%porosity and significantly reduced sintering time.The improved sintering can be explained by the presence of Y_(2)O_(3)and Nd_(2)O_(3)oxide layers,which form spontaneously on the surface of WE43 powder used in BJAM.These layers appear to be crucial in preventing shape distortion of the resulting samples and in enabling the development of sintering necks,particularly under sintering conditions exceeding the liquidus temperature of WE43 alloy.Sintered WE43 specimens rendered by BJAM achieved significant improvement in both corrosion resistance and mechanical properties through reduced porosity levels related to the sintering time.

Physical,mechanical and thermal properties of vacuum sintered HUST-1 lunar regolith simulant

Establishing a base on the Moon is one of the new goals of human lunar exploration in recent years.Sintered lunar regolith is one of the most potential building materials for lunar bases.The physical,mechanical and thermal properties of sintered lunar regolith are vital performance indices for the structural design of a lunar base and analysis of many critical mechanical and thermal issues.In this study,the HUST-1 lunar regolith simulant(HLRS)was sintered at 1030,1040,1050,1060,1070,and 1080℃.The effect of sintering temperature on the compressive strength was investigated,and the exact value of the optimum vacuum sintering temperature was determined between 1040 and 1060℃.Then,the microstructure and material composition of vacuum sintered HLRS at different temperatures were characterized.It was found that the sintering temperature has no significant effect on the mineral composition in the temperature range of 1030-1080℃.Besides,the heat capacity,thermal conductivity,and coefficient of thermal expansion(CTE)of vacuum sintered HLRS at different temperatures were investigated.Specific heat capacity of sintered samples increases with the increase of test temperature within the temperature range from-75 to 145℃.Besides,the thermal conductivity of the sintered sample is proportional to density.Finally,the two temperatures of 1040 and 1050℃were selected for a more detailed study of mechanical properties.The results showed that compressive strength of sintered sample is much higher than tensile strength.This study reveals the effects of sintering temperature on the physical,mechanical and thermal properties of vacuum sintered HLRS,and these material parameters will provide support for the construction of future lunar bases.

Magnetic properties and microstructures of terbium coated and grain boundary diffusion treated sintered Nd-Fe-B magnets by magnetron sputtering

Tb coating on the surface of commercial sintered Nd-Fe-B magnet was prepared by DC magnetron sputtering.The secondary heat treatment was used to regulate the microstructure for the enhancement of coercivity,namely diffusion treatment and annealing treatment.The coercivity increases significantly from 18.3 to 28.0 kOe,the remanence decreases slightly from 14.1 to 14.0 kGs,and the comprehensive magnetic properties are higher than 75(Hcj+(BH)_(max)=76.7).SEM results indicate that,on the one hand,950℃is the optimal diffusion temperature.Lower diffusion temperature results in insufficient diffusion of Tb element.Higher diffusion temperature can lead to the main phase grain growth,the decrease of Nd-rich phase,and forming holes in the magnet.On the other hand,500℃is the optimal annealing temperature.Lower annealing temperature can result in the reduction of Nd-rich phase.Higher annealing temperature can generate the non-defined Nd-rich thin layer between grains.

Enhancement of corrosion resistance in sintered Nd-Fe-B permanent magnet doping with different CuZn5 contents

Nd-Fe-B permanent magnets doped with CuZn5 powders were prepared via conventional sintered method. The effects of CuZn5 contents on magnetic properties and corrosion resistance of the magnets were sys- tematically studied. It shows that the remanence, coercivity, and maximum energy product decrease gradually with the increase in CuZn5 doping content. The magnet＇s corrosion kinetics in autoclaves environment and its electrochemical properties in electrolytes were also examined. It is interesting to see that the weight loss of 3.5 wt% and 4.5 wt% CuZn5 powders doping magnets is only 1 and 0 mg.cm^-2 after autoclaves test at 121 ℃, 2 × 10^5 Pa for 500 h, respectively, which is much lower than that of the magnets without CuZn5 doping. Electrochemical results show that the CuZn5 powders doping magnets display more positive corrosion potential （Eoorr） and lower corrosion current density （Icorr） than those of the original magnets without CuZn5 doping in sulphuric acid electrolyte and distilled water. It is, therefore, concluded that doping CuZn5 powders is a promising way to enhance the corrosion resistance of sintered Nd-Fe-B magnets.

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.

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.

Recycle for Sludge Scrap of Nd-Fe-B Sintered Magnet as Isotropic Bonded Magnet

The reduction diffusion method was performed for the sludge scrap of Nd-Fe-B sintered magnets with adding Ca metal to recover the oxidized Nd-Fe-B phase. After washing the resultant powders to remove Ca metal component, the powders obtained were recycled as an isotropic magnetic powder by the melt spinning method. The magnetic properties of powders as recycled were inferior, especially for the coercivity value, due to the deletion of rare earth metals during the washing process. The adjustment of metal composition, i.e., the addition of Nd metal, at the melt spinning process improved the magnetic properties to be B r=～0.75 T, H cj=～0.93 mA·m -1, and (BH) max=～91 kJ·m -3. The magnetic properties of the bonded magnets prepared from the composition-adjusted powders were B r=～0.66 T, H cj=～0.92 mA·m -1, and (BH) max=～70 kJ·m -3, which are approximately comparable to the commercially available MQPB boned one (B r=～0.73 T, H cj=～0.79 mA·m -1, and (BH) max=～86 kJ·m -3).

Microstructure and magnetic properties of sintered Nd-Fe-B magnets with Ce substitution for Nd by intergranular-alloy method

Aiming at the comprehensive utilization of the rare-earth resources and the preparation of the high-performance low-cost Nd-Fe-B magnets,sintered magnets with different Ce substitution amounts of 17.2 wt%,24.8 wt%and 31.8 wt%were prepared by intergranularalloy method.The influence of substitution of Ce for Nd on their microstructure and magnetic properties in this work was detailedly investigated.The results indicated that the remanence(Br)and the maximum energy product((BH)max)of the sintered magnets decreased monotonic ally with the increase in Ce substitution.However,the obvious enhancement of coercivity(Hcj)was also observed,which was mainly due to the improvement of microstructure and the smooth,continuous grain boundary(GB).It can be found that a reasonable Ce substitution of 24.8 wt%for the sintered magnets could promote the refinement of microstructure,leading to the realization of superior magnetic properties.It is expected that the investigations could be beneficial to offer a feasible method for preparing the high-performance low-cost Ce-doped magnets.

Improved corrosion resistance and thermal stability of sintered Nd-Fe-B magnets with holmium substitution

The effects of Ho substitution for Nd on the microstructure, corrosion resistance and thermal stability of the Nd-Fe-B magnets were investigated. The（Nd,Ho）-O phase was formed with increasing Ho substitution. The results of potentiodynamic polarization and highly accelerated stress test show improved corrosion resistance with increasing Ho substitution. The optimum mass loss 0.29 mg/cm^2 is achieved.Moreover, the average temperature coefficients for remanence and coercivity in the range of 25-150℃are both closer to zero, indicating improved thermal stability. The mechanisms for the improved corrosion resistance and thermal stability are discussed in relation to the microstructure featuring the（Nd,Ho）-O phase.