Effect of grain boundary diffusion of terbium on mode of mechanical fracture of sintered NdFeB magnets

Grain boundary diffusion process(GBDP) is a widely used method of increasing the coercivity of sintered NdFeB magnets.In this study,the effects of the GBDP on the bending strength and microhardness of sintered NdFeB magnets and the fracture mode were investigated.Results show that the bending strength of magnets is reduced by pickling and heat treatment and greatly recove rs after heavy rare earth element(Tb) grain boundary diffusion.The pickling and the heat treatment cause a slight decrease in...     

Recent progress of grain boundary diffusion process for hot-deformed Nd-Fe-B magnets

Grain boundary diffusion process(GBDP) was first proposed for sintered Nd-Fe-B magnets to achieve the high utilization efficiency of heavy rare earth elements.Recent success of fabricating high performance nanocomposite magnets by GBDP indicates that this method also exerts huge applicable potential on hot-deformed Nd-Fe-B magnets.In this review,the development and magnetic property enhancement mechanisms of different diffusion methods proposed on hot-deformed magnets were thoroughly elucidated....     

Diffusion Coefficient of Lanthanum in Al-Cu Alloy

In molten salt media,the rate of mass transfer process is slower than that of the charge transfer processof an electrochemical reaction.This is attributed to the high temperature which can propagate the rate of thecharge transfer process.Being the slowest,the diffusion process is the rate determining step in anelectrochemical reaction.The diffusion coefficient of lanthanum in Al-Cu alloy is determined byelectrochemical method,which will provide very important data for the study of co-deposition of lithiumwith rare earth ions in fused chlorides.     

Effect of annealing temperature on magnetic properties of a sintered Nd-Fe-B magnet after grain boundary diffusion with Dy70Cu30 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 Dy₇₀Cu₃₀ alloy.After GBDP the low eutectic temperature of the grain boundary phases decreases from the initial ...     

Influence of Al/Cu content on grain boundary diffusion in Nd-Fe-B magnet via in-situ observation

The influence of aluminum and copper content in the starting Nd-Fe-B magnet on grain boundary diffusion process(GBDP) was studied by observing the phase transformation behaviors of the magnets in-situ at high temperature. A higher coercivity increment is discovered in the sample with higher AI/Cu despite the fact that its Dy diffusion amount is the same as the other. DSC analysis shows an evident melting behavior in the higher Al/Cu sample. Laser scanning confocal microscopy(LSCM) in-situ characterization shows a large amount of melted intergranular phase spills out to the surface simultaneously at around 600 ℃ in the high Al/Cu sample, while the phase spills out gradually one after another in the range between 623 and680 ℃ in the other sample, which indicates that the intergranular phase can be more easily melted in the sample containing more AI/Cu. The area fraction of matrix phase remarkably shrinks while that of intergranular phase enlarges after LSCM heating, which demonstrates the outer region of the Nd_2 Fe_(14)B grains melt at the temperature of 900 ℃. Electron probe microanalyzer result(EPMA) shows that the Nd and Dy concentrate in edge regions and subsequently mix into the intergranular phase with the melting of the grain edge, while a large amount of AI and Cu in the intergranular phase spill out. Nevertheless, the sample with higher starting AI/Cu still remains higher residual contents after LSCM experiments, and that could probably be the main reason why the high AI/Cu magnet shows smaller coercivity decrement after LSCM experiment. Overall, the increase of AI/Cu in the starting magnet optimizes the Dy distribution and the wettability of intergranular phase, enhancing coercivity increment effect further.     

Electrochemical behavior of Ce（III） in LiF-BaF2 melts

The electrochemical behavior of Ce(III) was investigated in the molten LiF-BaF2 (81 mol.%-19 mol.%) on a molybdenum elec-trode in the temperature range of 1098-1188 K using cyclic voltammetry and chronopotentiometry. It was observed that CeF3 could be re-duced into cerium metal in a reversible one-step process exchanging three electrons (Ce(III)+3e-→Ce(0)) at the operating temperatures on a molybdenum cathode. The electrochemical reduction process was controlled by the diffusion of Ce(III) in the solution. The Ce(III) diffusion coefficients were calculated at different temperatures and the values obeyed the Arrhenius law with an activation energy of 87.5 kJ/mol.     

Effect of Tb(Ⅲ) on activity and stability of nattokinase

Nattokinase, is an effective fibrinolytic enzyme with the potential for fighting cardiovascular disease. The aim of study was to investigate the interaction of Tb(Ⅲ) with nattokinase and the impact of Tb(Ⅲ) on the enzyme activity and protein stability. The binding of Tb(Ⅲ) with nattokinase was studied by fluorescence spectrum in 100 mmol/L Tris-HCl(pH 8.0). It could be seen that the protein bound one Tb(Ⅲ) with low affinity, and the binding constants K were 2.90×10~4 L/mol at 288 K. Although the activity of nattokinase determined by tetra-peptide substrate method at proper pH and temperature was not influenced for the binding of Tb(Ⅲ), the transformation rate of substrate was increased to 113%. To better assess the stability of protease in the absence and presence of Tb(Ⅲ), nattokinase was unfolded through continuous concentrations urea. Based on the model of structural element, the results showed that Tb(Ⅲ) could not change the average structural element free energy ?G~0 element(H_2O) of nattokinase by the measurement of enzyme activity, but it could improve the stability of the global protein by the fluorescence spectral measurement.     

Numerical Simulation on Carburizing and Quenching of Gear Ring

 The carburizing process of the gear ring was simulated by taking into account the practical carburizing and quenching techniques of the gear ring and by solving the diffusion equation. The carbon content distribution in the carburized layer was obtained. Based on the results, the quenching process of the gear ring was then simulated using the metallic thermodynamics and FEM; it was found that the carburization remarkably affects the quenching process. Microstructures and stress distributions of the gear ring in the quenching process were simulated, and the results are confirmed by experiments.     

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.     

Oxidation Kinetics,Structural Changes and Element Migration during Oxidation Process of Vanadium-titanium Magnetite Ore

The oxidation kinetics,structural changes,and elements migration during the oxidation process of the vanadium-titanium magnetite(VTM)ore were analyzed.Kinetics analysis indicated that the oxidation process was controlled by diffusion control and could be divided into interface diffusion and lattice diffusion with apparent activation energy of 99.69kJ/mol and 144.08kJ/mol in the range of 800-1 000 ℃,respectively.The surface structure changed with the oxidization temperature as follows:dense surface→nano-sized sheets→submicron particles→molten particles.The compact structure changed into porous one because of the elements migration and enrichment.Both Fe and Ti elements migrated in the opposite direction during the oxidation process.The V element in the raw ore stably existed in the form of V~(5+)state,some vanadium migrated and occupied the tetrahedral sites of the hematite during the oxidation process.     

晶界扩散Tb对烧结Nd-Fe-B组织与磁性能的影响

用磁控溅射法在烧结Nd-Fe-B磁体表面沉积Tb金属薄膜并进行晶界扩散处理,对比经不同热扩散温度及时间处理后的磁体组织和磁性能变化.结果 表明,925℃×10 h+500℃×2 h为最佳晶界扩散工艺,可将磁体矫顽力提高到1630.9 kA· m-1,较原始磁体提升50％,同时剩磁和磁能积无明显下降,磁体仍具有较高的退磁...     

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 ...     

Coercivity enhancement mechanism of grain boundary diffused Nd-Fe-B sintered magnets by magnetic domain evolution observation

The grain boundary diffusion(GBD) technology was used to prepare high performance Nd-Fe-B sintered magnets by NdH_3 and TbH_3 nanoparticle diffusion.The factors affecting the coercivity of GBD magnets include distribution of rare earth rich grain boundary phase and substitution of the heavy rare earth.In order to distinguish the influence of various factors on the coercivity,the microstructure and magnetic domain evolution of the original,reference,Nd-diffused,and Tb-diffused magnets were analyzed.The core-shell structure formed by heavy rare earth substitution is the main factor of coercivity enhancement,and it can transform the magnetic domain reversal mode from easy-nucleation(EN) to difficultnucleation(DN).With increasing the diffusion depth,the shell of the core-shell structure gradually becomes thinner,DN grains gradually decrease while the EN grains gradually increase,indicating that the magnetic domain reversal mode is directly related to the core-shell structure.     

Improvement of coercivity and corrosion resistance of Nd-Fe-B sintered magnets by doping aluminium nano-particles

Nd-Fe-B permanent magnets with a small amount of Al nano-particles doping were prepared by conventional sintered method. Effect of Al content on magnetic property, corrosion resistance and oxidation properties of the magnets were studied. Investigation showed that the coercivity rose gradually, while the remanence decreased simultaneously with increase of Al doping amount. Further investigation revealed that most Al element diffused into the main phase and some Al element diffused into the Nd-rich phase. The autoclave test results showed that the corrosion rate of the magnets decreased with Al content increasing. After oxidation, the maximum energy product losses of the magnets with 0.0 wt.% and 0.2 wt.% Al nano-particles doping were 6.13% and 3.99%, respectively. Therefore, Al nano-particles doping was a promising way to enhance the coercivity and corrosion resistance of sintered Nd-Fe-B magnet.     

Influence of dysprosium substitution on magnetic and mechanical properties of high intrinsic coercivity Nd-Fe-B magnets prepared by double-alloy powder mixed method

The double-alloy powder mixed method is very proper for developing new small-mass products by changing the composition of sintered Nd-Fe-B magnets, and there is little research on this aspect. The variation on magnetic and mechanical properties of high intrinsic coercivity Nd-Fe-B magnets prepared by double-alloy powder mixed method was discussed, which is a method blending two-type main phase alloy powders with different components. The results showed that the intrinsic coercivity and density of sintered Nd-Fe-B magnets increased gradually with the increase in Dy content, and the double-alloy powder mixed method could obtain high intrinsic coercivity Nd-Fe-B magnets with good crystallographic alignment and microstructure. The bending strength of sintered Nd-Fe-B magnets declined, and the Rockwell hardness of sintered Nd-Fe-B magnets first declined, and then increased with the increase in Dy content. The microstructure showed that there existed the phenomenon that the Dy element diffused into main phase during sintering process, and the distribution of Dy content in main phase had some variation in homogeneity as a result of incomplete reaction between the double-alloy powder types.     

Improvement of microstructure and coercivity for Nd-Fe-B sintered magnets by boundary introducing low melting point alloys

Different from the grain boundary diffusion process(GBDP),which is suitable for modifying thin magnet,a green-pressing agents permeation process(GAPP) that uses low melting point alloys was applied to the Nd-Fe-B green compact with a thickness over 15 mm to reconstruct the boundary microstructure of a sintered Nd-Fe-B magnet.The coercivity increases from 12.3 kOe for the sample free of Pr_(80)Al_(20) to16.8 kOe for the sample with 2 wt% Pr_(80)Al_(20).By further increasing the Pr_(80)Al_(20) content to 3 wt%,the coercivity increases slightly,but the remanence and H_k/H_(cj) deteriorate obviously.The optimal comprehensive properties of H_(cj)=16.8 kOe,B_r=13.4 kG and H_k/H_(cj)=0.975 are obtained at 2 wt% Pr_(80)Al_(20),since matrix phase grains are separated by relatively continuous thin grain boundary layers,which weaken the magnetic coupling between adjacent grains.The coercivities of the samples from the GAPP that use2 wt% Pr_(80)Al_(20),Pr_(70)Al_(30) and Pr_(60)Tb_(20)Al_(20) alloys,respectively,can be enhanced to a large extent.However,the coercivity of the magnet reconstructed with Pr_(80)Al_(20) is lower than that of the sample with Pr_(60)Tb_(20)Al_(20) but is higher than that of the sample reconstructed with Pr_(70)Cu_(30) alloy.Moreover,the coercivity of the sample from the GAPP using 2 wt% Pr_(80)Al_(20) is much higher than that of the sample from the GBDP,which is due to a nearly uniform boundary microstructure from the surface to the interior of the thick magnet from the GAPP,thus providing new insights into the fabrication of thick and bulky permanent magnets with high coercivity.     

Effects of grain boundary diffusion process on magnetic properties enhancement and microstructure evolution of hot-deformed Nd-Fe-B magnets

Grain boundary diffusion(GBD) process is an important approach for producing Nd-Fe-B magnets with high coercivity and high thermal stability.The GBD for hot-deformed Nd-Fe-B magnets with nanocrystalline micro structure is more complicated compared to sintered magnets.Here,we investigated the effects of different GBD methods,i.e.,intergranular addition(in-situ GBD 1#),in-situ GBD from magnet surface during hot pressing and hot deformation(in-situ GBD 2#),and conventional GBD,on the magnetic prope...     

Effect of niobium on thermal stability and impact toughness of Nd-Fe-B magnets with ultra-high intrinsic coercivity

The effects of Nb on the thermal stability and impact toughness of ultra-high intrinsic coercivity of Nd-Fe-B magnets were investigated.The results showed that the addition of Nb could improve the thermal stability,and obviously increased the impact toughness of sintered Nd-Fe-B magnets.The optimum thermal stability of sintered Nd-Fe-B magnets was obtained when the content of Nb was 1.0 at.%.The maximum impact toughness of sintered Nd-Fe-B magnets was obtained when the content of Nb was 1.5 at.%,but the magnetic properties of sintered Nd-Fe-B magnets drastically deteriorated when the content of Nb increased from 1.0 at.% to 1.5 at.%.The microstructure showed that overfull Nb addition made many ultra-fine grains get together,which led to the density of sintered Nd-Fe-B magnets decline and drastically deteriorated the magnetic properties of sintered Nd-Fe-B magnets.     

晶界扩散中Tb对烧结NdFeB磁体微观组织和磁性能的影响

通过晶界扩散技术提升烧结钕铁硼(NdFeB)磁体矫顽力的方法已获得广泛应用,为了研究重稀土磁粉对磁体综合磁性能的影响,本文采用喷涂扩散的方法将重稀土Tb含量为6.0%(质量分数)的磁粉作为复合扩散源的一部分进行晶界扩散并制备了高性能烧结NdFeB磁体。结果表明,当主扩散源占比为60%(质量分数)时,Nd₄₀Tb₆₀对应扩散磁体的矫顽力最高达到21.52 kOe,矫顽力增幅明显。经过微观组织结构和XRD表征分析,重稀土元素Tb沿晶界相扩散进入磁体内部的同时发生了晶格取代反应,可在晶粒表层生成磁晶各向异性场更强的(Nd,Dy/Tb)₂Fe₁₄B硬磁相,显著增强了磁体矫顽力。当主扩散源占比为20%、40%和80%(质量分数)时,Nd₈₀Tb₂₀,Nd₆₀Tb₄₀和Nd₂₀Tb₈₀对应扩散磁体的矫顽力增幅较小,其中Nd₈₀Tb₂₀扩散...