Twinning,phase boundary structure and development of high coercivity in Fe-rich Sm2Co17-type magnets

The microstructure of twinning as well as the phase boundary between 1:5 H and 2:17 R phase in Fe-rich Sm₂Co₁₇-type magnets was characterized at atomic scale using nanobeam diffraction and highresolution STEM-HAADF imaging,and the reason for the dramatic increase of coercivity during slow cooling was investigated based on the microchemistry analysis.The twinning relationship in the 2:17 R phase originates from ordered substitution of Sm atoms by Co-Co atomic pairs on every three(3033)and(3033)planes,leading to formation of two corresponding equivalent twin variants.The basal plane of the 2:17 R phase,the 1:3 R platelet phase across the 2:17 R cell and the 1:5 H cell boundary phase between two adjacent 2:17 R cells all can act as effective twin boundary.The cell boundary phase is precipitated along the pyramidal habit plane,and a fully coherent phase boundary(PB)is formed between the 1:5 H and 2:17 R phases with the orientation relationship to be PB//(1121)1:5 H//(1011)₂:17 R.The phase boundary may either be parallel to or intersect with the pyramidal planes occupied by Co-Co atomic pairs.The substantial increase of coercivity during slow cooling is ascribed to the development of large gradient of the elements concentration within the cell boundary phase,resulting in large gradient of domain wall energy,and thus the pinning strength of the cell boundary phase against magnetic domain wall motion is significantly enhanced.     

Magnetic properties and magnetization behavior of SmCo-based magnets with TbCu7-type structure

The nanocrystalline magnets with nominal compositions of Sm1-xLuxCo6.8Zr0.2(x=0,0.2,0.4,0.6)were prepared directly by the intensive milling.The effects of Lu content on the phase structure,the magnetic properties,and magnetization behaviors were also investigated.The XRD patterns of the as-milled samples showed a single SmCo7 phase with TbCu7 structure.Lu addition was proved to result in relevant improvements in the microstructure and magnetic properties,especially in the maximum energy product(BH)max.It was shown that a higher maximum energy product and coercivity of about 17.47 kJ/m3 and 473.45 kA/m were obtained in the sample with x=0.2.From the analysis of the magnetization reversal behavior,it was found that a stronger intergrain exchange coupling interaction was observed in the samples with Lu-doping.From the studies of the coercivity mechanism,it was shown that nucleation model was the dominant magnetization reversal process at the elevated temperature.     

Effect of niobium addition on magnetization reversal behavior for SmCo-based magnets with TbCu7-type structure

The effect of Nb addition on the microstructure and magnetic properties of nanocrystalline Sm(CobalNbxZr0.02)7 permanent magnet were investigated. The magnetization reversal behavior for ball milled Sm(CobalNbxZr0.02)7 samples with high coercivity was investigated by analyzing hysteresis curves and recoil loops of demagnetization curves. Nb addition proved to result in relevant improvement in the magnetic properties, especially in the coercivity Hc. It was shown that the magnetic properties of Sm(CobalNbxZr0.02)7 nanocrystalline magnets were improved by an additional 0.06 at.% Nb. In particular, Hc was improved from 602 to 786 k A/m at room temperature. The maximum value of the integrated recoil loops area for 0.06 at.% Nb-doped samples of 1.81 k J/m3 was much lower than that of the Nb-free sample, which could be explained by a smaller recoverable portion of the magnetization remaining in the Nb-doped sample when the applied field was below the coercivity Hc. The nucleation field Hn for irreversible magnetization reversal of the magnetically hard phase were calculated by analyzed in terms of the ΔMirrev-H curve and the Kondorsky model.     

Effect of Terbium addition on the coercivity of the sintered NdFeB magnets

The effects of Tb addition on the microstructure and magnetic properties of the NdFeB magnets prepared by HD method were investigated by X-ray diffraction(XRD) and BH magnetometers.The results of the microstructure showed that both the Tb-doped and undoped permanent magnets were composed mostly of Tetragonal phase Nd2Fe14B(space group P42/mnm) and a trace amount of Nd-rich phase.Accordingly,addition of Tb led to a decrease of the pole density factor of(004),(006) and(008) crystal plane of the Nd2Fe14B phase calculated by Horta formula,but the coercivity of the magnets increased from 2038 kA/m up to 2302 kA/m as a consequence of Tb addition.The study of the Hc(T)/Ms(T) versus/Ms(T) behavior showed that the nucleation was the dominating mechanism for the magnetization reversal in both sintered magnets,and the microstructural parameters of αk and Neff were obtained also.The Kronmüller-plot showed an increase of the αk responsible for an increase of the coercivity.     

Coercivity kinetics upon step annealing of sintered Sm(Co_(0.88-x)Fe_xCu_(0.09)Zr_(0.03))_7 magnets

Behavior of the coercivity of the high-temperature Sm(Co_(0.88-x)Fe_xCu_(0.09)Zr_(0.03))_7 magnets depending on the temperature and time of annealing with the temperature decreasing stepwise from 700 to 400℃ was investigated.It is shown that the growth rate of coercivity abruptly increases at the initial stage of annealing in the vicinity of the Curie temperature of the SmCo_5 phase.The origin of the effect is the counter diffusion of Cu and Co atoms through dislocation tubes,which form because of enhanced stresses and a partial breakage of coherent coupling at the interface of the Sm_2 Co_(17) and SmCo_5 phases.Diffusive enrichment of the SmCo_5 phase in Cu close to the interface with Sm_2 Co_(17) leads to relaxation of stresses and increases in the gradient of the magnetic domain-wall energy and coercivity.     

Analysis of Rolling Pressure in Asymmetrical Rolling Process by Slab Method

 The plane strain asymmetrical rolling was analyzed using slab method. The contact arc was replaced by parabola, and the constant surface friction status was adopted during the analysis. The deformation area was divided into three zones according to the direction of the friction. Then, the three zones were studied, respectively. A rolling force model and a rolling torque model were developed based on the analysis, and they were used to analyze the influence of asymmetrical rolling factors on deformation area and unit pressure if they had good precision which was determined by comparing the calculated results with the measured ones.     

Computer Simulation of Microstructure Evolution of 82B Rod at Different Cooling Rates

According to thermodynamics and kinetics of phase transformation,a mathematical model of phase transformation was proposed,and the microstructure evolution of an 82B rod at different cooling rates was simulated by using the FEM software Marc/Mentat,based on the measurement of time-temperature transformation（TTT）curves of the 82B rod.The simulated results were in good agreement with the actual measurements.From the results of computer simulation it was found that the cooling rate of the 82B rod,after laying,should be controlled within 5-8 ℃/s.In the microstructure of rod there were over 95% of pearlite volume fraction and a small quantity of dispersive martensite（less than 5%）.     

Dynamic Water Modeling and Application of Billet Continuous Casting

The continuous casting process is used for solidifying molten steel into semi-finished steel.The technology of secondary cooling is extremely important for output of the casting machine and billet quality.A dynamic water model was introduced,including solidification model in the secondary cooling,feedforward control strategy based on continuous temperature measurement in tundish,and feedback control strategy based on surface temperature measurement.The mathematical model of solidification process was developed according to the principle of solidification,and the solidification model was validated by measuring billet shell thickness through shooting nail and sulfur print.Primary water distribution was calculated by the solidification model according to procedure parameters,and it was adjusted by the other two control strategies online.The model was applied on some caster and billet quality was obviously improved,indicating that the dynamic water model is better than conventional ones.     

Effect of chromium interlayer on magnetic exchange coupling of SmCo/Cr/TbFeCo multilayer thin films

A series of SmCo/Cr/TbFeCo multilayer thin films with perpendicular anisotropy were prepared by RF- magnetron sputtering system, and the effects of Cr interlayer thickness on magnetic properties and interlayer exchange coupling were investigated. It was found that the magnetic properties varied with the thickness of Cr interlayer, especially the values of saturation magnetization Ms and the coercivity Hc fluctuated periodically with the thickness of Cr interlayer. STM images revealed that the variation of coercivity Hc was attributed to the microstructure change of SmCo layer influenced by Cr interlayer, and the variation of Ms was related to interlayer exchange coupling.     

Influence of Zr Additions on Microstructure and Magnetic Properties of Nanocomposite Nd10.5Fe78-xCo5ZrxB6.5（x=0-5） Alloys

The influence of Zr addition on the microstructure and magnetic properties of nanocomposite Nd10.5Fe78-x Co5ZrxB6.5(x=0-5)alloys was investigated. It was found that the intrinsic coercivity could be significantly improved by the addition of 2% (atom fraction) Zr. The presence of small amount of amorphous phase is responsible for tile low intrinsic coercivity for Zr-free alloy. The small amount addition of Zr may suppress the growth of grains of α-Fe and Nd2Fe14B phases. The more homogeneous microstrueture with an average grain size of 20 nm can be obtained for Nd10.5 Fe76 Co5Zr2B6.5 alloy.     

Sm2Co17永磁体的显微组织及其对矫顽力的影响

探讨了Sm(CobalFe0.197Cu0.049Zr0.026)7.5,Sm(CobalFe0.197Cu0.062Zr0.034)7.5永磁体的显微组织及其对矫顽力的影响.Sm2Co17永磁体由2:17相和1:5相两相所形成的胞状组织构成,并影响材料矫顽力的大小.在高矫顽力磁体的单晶表面有大量取向一致的沟痕,而不同晶粒内部的沟痕取向不同;沟痕较多时,磁体内所形成的1:5相增多,对畴壁的钉扎能力增强,有利于内禀矫顽力的提高.磁体表面的白色物质含Sm较多时可降低矫顽力.     

Investigation on Hard Magnetic Properties of Nanocomposite Permanent Magnets with Precipitate-Typed Microstructure by Micromagnetic Finite-Element Methods

Maximumenergyproduct (BH) maxisakeychar acteristicofapermanentmagnet (PM ) .Theoptimal(BH) maxislimitedbythevalueofJr2 / 4 μ0 (Jrrema nence)correspondingtoanidealrectangularhysteresisloopwhencoercivityμ0 HcisatleastlargerthanJr/ 2 .FormostrareearthPM ,thecoercivityisfarlargerthantheremanence[1,2 ] .Thus ,remanenceenhance mentbecomesanimportantroleindeveloping(BH) max.Sincehighremanencewasfoundinisotrop icnanostructuredPM ,muchefforthasbeenpaidtoachievehighperformancePM[3,4 ] .Thehigh…     

Effects of copper and zirconium contents on microstructure and magnetic properties of Sm(Co,Fe,Cu,Zr)_z magnets with high iron content

The evolution of the microstructure,microchemistry and magnetic properties of the Sm(Co_(bal)Fe_(0.28)-Cu_yZr_x)_(7.6) magnets with different Zr and Cu contents was investigated.It is found that the coercivity of the Sm(Co,Fe,Cu,Zr)_z magnets is sensitive to Zr content.The deficiency of Zr content causes heterogeneity of Cu and Fe distributions,while an excessive Zr content leads to the formation of a SmCoZr impurity phase.The cellular structure and distribution of Cu concentration.gradient between the cell boundary phase and cell pha se are destroyed by inappropriate Zr content,which results in a reduction of coercivity.The Cu concentration difference between the cell boundary phase and cell phase increases with increasing Cu content.The coercivity of the Sm(Co_(bal)Fe_(0.28)Cu_yZr_(0.02))_(7.6) magnets increases from 10.4 to 25.4 kOe for y=0.05 and y=0.07.However,the excess of Cu element destroys the cell boundary phase and enlarges the cell size,resulting in a significant decrease of squareness and energy density.The optimum performance(remanence of 11.4 kG,coercivity of 2 5.4 kOe,maximum magnetic ene rgy product of 30.4 MGOe) was obtained for the Sm(Co_(0.63)Fe_(0.28)Cu_(0.07)Zr_(0.02))_(7.6) magnet.     

Microstructure improvement related coercivity enhancement for sintered NdFeB magnets after optimized additional heat treatment

The microstructure, especially the Nd-rich phase and the grain boundary, in sintered NdFeB magnets plays an important role in magnetic reversal and coercivity mechanism. To better understand the effects of the microstructure on the coercivity, we investigated the microstructure and properties improvements of a commercial sintered NdFeB magnet after optimized additional heat treatment. The coercivity is enhanced from 1399 to 1560 kA/m. This enhancement has been explained in terms of the evolution of the grain boundary structure, and the formation of continuous thin layers of Nd-rich phase is important for high coercivity. The micromagnetic simulation together with the numerical analysis based on the nucleation model suggest that the reversed magnetic domains nucleate mainly at the interface of multi-junctions of Nd₂Fe₁₄B grains with high stray fields during the demagnetization process. Both improved anisotropy fields at grain boundaries and reduced stray fields at multi-junction Nd-rich phases contribute to the coercivity enhancement. This work has importance in understanding the crucial microstructure parameters and enhancing the obtainable properties for sintered NdFeB magnets.     

高矫顽力2:17型SmCo永磁合金的显微组织分析

制备了具有高矫顽力的2:17型SmCo磁体,采用透射电子显微镜对所制得的具有高矫顽力、低温度系数的2:17型磁体的微观组织进行了研究。结果表明:该磁体具有胞状显微组织,胞内为菱方结构的2:17相,胞壁为六方结构的1:5相,具有六方结构的2:17相位于胞状组织的内部;整齐、完整的胞状组织是获得高性能磁体的必要条件;胞状组织的尺寸大小和各元素在各相中的分布是决定矫顽力大小的关键因素。     

Effects of Pr-Cu-Ti intergranular addition on microstructure and magnetic properties of heavy-rare-earth-free Nd-Fe-B sintered magnets

By intergranular addition of Pr-Cu-Ti alloy powders in the Nd-Fe-B sintered magnets with the normal B component, we propose an approach to the optimization of grain boundary and local Nd-Fe-B composition system. The coercivity is enhanced from 1.42 to 1.86 T, while further addition leads to a reduction in remanence and coercivity. The analyses of phase composition reveal that Ti mainly exists in the form of metallic Ti alloy, and part of Ti combines with B to form the TiB₂ phase after the liquid phase sintering process. This process results in a consumption of B in the local Nd-Fe-B composition system and a change of the grain boundary component, which contributes to the formation process of the RE₆(Fe,M)₁₄ phase after the annealing process. Therefore, with the modification of grain boundary and composition system, the intergranular addition of Pr-Cu-Ti induces the generation of continuous thin grain boundary phases. It promotes the intergrain exchange decoupling, increasing the coercivity in the annealed magnet. While the excess addition results in the segregation of TiB₂, as well as the precipitation of TiB₂ into the Nd-Fe-B phase, which leads to structural defects. Thus, the further effort for the addition alloy with Ti to reduce the deterioration of the microstructure will lead to further improvement in magnetic properties.     

Influence of Zr Additions on Microstructure and Magnetic Properties of Nanocomposite Nd10.5Fe78-xCo5ZrxB6.5 (x=0～5) Alloys

The influence of Zr addition on the microstructure and magnetic properties of nanocomposite Nd10.5Fe78-xCo5ZrxB6.5 (x=0～5) alloys was investigated. It was found that the intrinsic coercivity could be significantly improved by the addition of 2% (atom fraction) Zr. The presence of small amount of amorphous phase is responsible for the low intrinsic coercivity for Zr-free alloy. The small amount addition of Zr may suppress the growth of grains of α-Fe and Nd2Fe14B phases. The more homogeneous microstructure with an average grain size of 20 nm can be obtained for Nd10.5Fe76Co5Zr2B6.5 alloy.     

Effects of pre-aging on defects evolution and magnetic properties of Sm-Co-Fe-Cu-Zr magnets

The heterogeneous precipitation in the 2:17-type Sm-Co-Fe-Cu-Zr permanent magnets has been found to contain complex formation and dissociation of defects. Though low-temperature pre-aging has been utilized to promote the precipitate nucleation by the enlarged chemical driving force, how the defects evolve after pre-aging and how the possibly changed defects state affects the subsequent precipitation behavior remain unclear. In this work, a model magnet Sm₂₅Co_47.9Fe_18.5Cu_5.6Zr_3.0 (wt%) was selected to study. Through comparison with the as-solution-treated state, it is found that pre-aging for 2 h at 550 °C reduces the defects density, which was characterized by less cell boundaries (i.e., larger cell size) and less basal stacking faults inside the cells (i.e., higher 2:17R ordering degree). Further studies reveal that after aging for the same time (10 h) at the same temperature (830 °C), the reduced density of defects by pre-aging also leads to slower precipitation/phase transformation kinetics when compared with the non-pre-aged one, which was characterized by the lower 2:17R ordering degree and smaller coercivity for the former. These findings suggest that pre-aging has a strong influence on the density of defects and their evolution during subsequent isothermal aging process, which should be carefully considered to tailor the microstructure and magnetic properties of Sm-Co-Fe-Cu-Zr magnets.     

Effects of Nd–Ga intergranular addition on microstructure and magnetic properties of heavy-rare-earth-free Nd-Fe-B sintered magnets

In this study, we propose an approach of grain boundary modification that can significantly increase the coercivity of the B-lean Nd-Fe-B sintered magnets by intergranular addition of Nd–Ga. The coercivity is substantially enhanced from 1.51 to 2.04 T through optimizing the microstructure and adjusting the phase composition for the grain boundary phase in the annealed magnets. The matrix grains are covered by a continuous thin grain boundary phase accompanying the formation of intermetallic Nd₆Fe₁₃Ga phases. The analysis of magnetic behaviors above Curie temperature confirms that the grain boundary phase of annealed Nd–Ga doped magnets appears to be non-ferromagnetic, facilitating the intergrain exchange decoupling. Microstructure observation in grain boundary area indicates that some surface of the matrix grain is dissolved in the formation process of the Nd₆Fe₁₃Ga phase. It gives rise to a decrease in the proportion of matrix grains and saturation magnetization of the magnet. The detailed relationship between magnetic properties and microstructure is discussed based on these results.     

Y取代对Pr-Nd-Fe-B合金微观结构和磁性能的影响

基于熔体快淬技术，研究了不同Y取代量对[（Pr_0.25Nd_0.75）_1-xY_x]_13.9Fe_80.1B₆合金物相组成、磁性能、晶间磁相互作用和微观结构的影响.结果表明，适量Y替代Pr、Nd元素，可以抑制Fe₃B相的形成，且合金矫顽力温度稳定性增强.当Y取代Pr、Nd元素的量为30 %时，居里温度仅轻微从307 ℃下降至302 ℃. Y取代具有一定程度的晶粒细化作用，有助于改善合金的微观结构.此外，Y取代还可以增强主相晶粒间的交换耦合作用.