Structure and Magnetic Properties of Sm2Fe17Nx Sintering Magnets Prepared by Spark Plasma Sintering

Bulk Sm2Fe17Nx sintering magnet was fabricated by spark plasma sintering(SPS) technique. The effects of sintering pressure and sintering temperature on the magnetic properties of the Sm2Fe17Nx magnet were investigated. As a result, the density of the magnet is obviously improved with the increase of sintering pressure, but the coercivity drops since Sm2Fe17Nx has decomposed into SmN, α-Fe and N2. When sintering temperature was only above 200 ℃ under 1 GPa sintering pressure, the coercivity even begins to decrease, which indicates that high pressure promotes the decomposition of the Sm2Fe17Nx at lower temperature. The decomposition is also proved by the decrease of nitrogen and increase of α-Fe in the magnets.     

Antioxidation Study of Sm（Co, Cu, Fe, Zr）z-Sintered Permanent Magnets by Metal Injection Molding

2∶17type Sm(Co ,Cu ,Fe ,Zr)zpermanent mag-nets originatedfromthe investigationinthe 1970s .Sm(Co ,Cu ,Fe ,Zr)zpermanent magnets have excellentintrinsic magnetic properties such as very high Curietemperature , high anisotropy fields , and relativelyhigh saturation magnetizations[1 ~4]. Hence the mag-nets play an i mportant role in national defence andmodernindustry .Because of the high brittleness of Sm(Co ,Cu ,Fe ,Zr)zpermanent magnets ,theirtransfor-mationinto complex,small ,precision …     

Sm2(Fe,M)17Nx稀土永磁材料的研究进展

综述了Sm2(Fe，M)17Nx永磁材料的最新研究进展，介绍了Sm2(Fe，M)17Nx磁粉及磁体的制备技术，说明用其他元素替换Sm或Fe对材料性能的影响，以及粉末颗粒具有最佳的尺寸和形貌的重要性。并指出放电等离子烧结技术(SPS)有望成为制备Sm2(Fe，M)17Nx致密磁体的一个有效方法。     

Magnetic Microstructures of 2：17 Type Sm（Co,Fe,Cu,Zr）z Magnets Detected by Magnetic Force Microscopy

The magnetic microstructures of 2：17 type Sm （Co, Fe, Cu, Zr）z magnets were detected by magnetic force microscopy. Comparing the microstructures of the specimens eoated with and without Ta thin film before and after heat-treatment, it is found that： （a） as a protection layer, Ta coating layer about 20 nm thick can effectively restrain Sm volatilization under high temperature; （b） the stress built in the 2.17 type Sm-Co magnets during specimen preparation only affects some local parts of the domain structures; （c） the magnetic microstructures vary largely for specimens heat-treated at high temperature without Ta film coating due to Sm volatilization. In addition, by comparing with high coercivity Fe-Pt point tips, it is found that the Co-Cr thin-film tips are not suitable for detecting the magnetic microstructures of strong permanent magnets.     

Magnetic Microstructures of 2:17 Type Sm(Co,Fe,Cu,Zr)z Magnets Detected by Magnetic Force Microscopy

The magnetic microstructures of 2:17 type Sm(Co,Fe,Cu,Zr)z magnets were detected by magnetic force microscopy.Comparing the microstructures of the specimens coated with and without Ta thin film before and after heat-treatment, it is found that: (a) as a protection layer, Ta coating layer about 20 nm thick can effectively restrain Sm volatilization under high temperature;(b) the stress built in the 2:17 type Sm-Co magnets during specimen preparation only affects some local parts of the domain structures;(c) the magnetic microstructures vary largely for specimens heat-treated at high temperature without Ta film coating due to Sm volatilization.In addition, by comparing with high coercivity Fe-Pt point tips, it is found that the Co-Cr thin-film tips are not suitable for detecting the magnetic microstructures of strong permanent magnets.     

Study on bulk Sm2 Fe17 Nx sintered magnets prepared by spark plasma sintering

Abstract

Sm₂Fe₁₇N_x sintered magnets were fabricated by spark plasma sintering (SPS) technique. Effects of sintering pressure, sintering temperature and heating rate on the magnetic properties and crystal structures of the magnets were investigated. The results showed that the density of the magnet was obviously improved with increasing sintering pressure, but the coercivity dropped simultaneously because Sm₂Fe₁₇N_x decomposed into SmN, α-Fe and N₂. The coercivity decreased rapidly when sintering temperature was above 200°C under 1 GPa sintering pressure, which indicated that high pressure promoted the decomposition of Sm₂Fe₁₇N_x even at low temperature. In addition, the decomposition could not be effectively restrained even if the heating rate reached 450°C min^?1.     

Sm2Fe17Nx稀土永磁材料的研究现状及进展

简要分析了Sm2Fe17Nx的晶体结构、内禀磁特性和N原子与磁性能的关系。着重介绍了Sm2Fe17Nx永磁材料的制备方法以及目前制备工艺存在的问题,并指出了其研究和发展趋势。     

Optimization of microstructures and magnetic properties of Sm(CobalFe0.227Cu0.07Zr0.023)7.6 magnets by sintering treatment

Magnetic properties and microstructures of Sm(Co_(bal)Fe_(0.227)Cu_(0.07)Zr_(0.023_)_(7.6) sintered magnets were optimized by sintering treatment. Results show that the knee-point magnetic field, Hknee, is twofold up and the intrinsic coercivity Hcjincreases by 40%, ranging from 21.64 to 30.39 kOe at the cost of a little decrease of Brfrom 10.84 to 10.31 kGs with sintering temperature decreasing from 1488 to 1473 K. And the average domain width is narrower and more uniform for the specimen sintered at 1473 K than that of the specimen sintered at 1488 K. It is impressive that the density of lamellar phase increases from ~0.050 to ~0.058 nm~(-1) with the sintering temperature decreasing from 1488 to 1473 K. Moreover, the average cellular size is about ~84 nm for the magnets sintered at 1473 K, which is 80% of that of the magnets sintered at 1488 K(~97 nm). And the cell boundary width of the magnets sintered at 1473 K(~7 nm) is only half average width of the magnets sintered at 1488 K(~14 nm). It is found that the Cu content in the cell boundaries is much higher(~17 at%) in the magnets sintered at 1473 K compared to that of the magnets sintered at 1488 K(~10 at%). It can be concluded that smaller cells and narrower cell boundaries together with higher gradient of Cu content are key points for obtaining the optimum Hkneeand Hcj.     

Synthesis mechanism of Sm₂Fe₁₇ alloy produced in reduction-diffusion process

Sm2Fe17 alloy was the precursor of Sm2Fe17Nx magnetic materials.Reduction-diffusion(R/D) method was a new preparation process for the Sm2Fe17 alloy,and had been widely employed as a new preparation method for rare earth-transition metal intermetallic compounds.In this text,thermodynamics and kinetics for the synthesis of the Sm2Fe17 alloy by reduction-diffusion(R/D) method in the Ca-Sm2O3-Fe system were analyzed.The related synthesis mechanism of this reaction was investigated in detail by means of scanning electron microscope(SEM).The results showed that the thickness of the Sm2Fe17 alloy layer versus the reaction time could be fit by the parabola law,and its growth model was determined to be:(L0-L)2=43.848 t,the diffusion of Sm into Fe proceeded with the formation of the Sm2Fe17 phase from the very beginning of the reaction,and rich samarium phases,such as SmFe2 and SmFe3,were not formed,and the rate-determining step of the R/D reaction was found to be the peritectic reaction between liquid samarium and solid iron.     

Improved Electrical Insulation of Rare Earth Permanent Magnetic Materials With High Magnetic Properties

 Rare earth permanent magnetic materials are typical electrical conductor, and their magnetic properties will decrease because of the eddy current effect, so it is difficult to keep them stable for a long enough time under a high frequency AC field. In the present study, as far as rare earth permanent magnets are concerned, for the first time, rare earth permanent magnets with strong electrical insulation and high magnetic performance have been obtained through experiments, and their properties are as follows: (1) Sm2TM17: Br=062 T, jHc=8037 kA/m, (BH)m=5897 kJ/m3, ρ=7 Ω·m; (2) NdFeB: Br=0485 T, jHc=76633 kA/m, (BH)m=3796 kJ/m3, ρ=9 Ω·m. The magnetic properties of Sm2TM17 and NdFeB are obviously higher than those of ferrite permanent magnet, and the electric insulating characteristics of Sm2TM17 and NdFeB applied have in fact been approximately the same as those of ferrite. Therefore, Sm2TM17 and NdFeB will possess the ability to take the place of ferrite under a certain high frequency AC electric field.     

Preparation and characterization of sodium silicate/epoxy resin composite bonded Nd-Fe-B magnets with high performance

As an organic binder for bonded Nd-Fe-B magnets, epoxy resin(EP) has poor heat resistance but good moisture resistance, while sodium silicate(SS) has poor moisture absorption but better heat resistance and corrosion resistance. In order to improve high temperature stability and decrease moisture absorption of bonded Nd-Fe-B magnets, EP/SS composites were applied as the binder to prepare bonded Nd-Fe-B magnets. The magnetic properties, moisture absorption, corrosion resistance, compressive strength and microstructure of composite bonded magnets were investigated. The results show that EP/SS bonded magnets can obtain excellent magnetic properties at room temperature, and even useable magnetic properties a thigh temperature environments at 200°C. EP/SS composite binder effectively improves heat resistance and corrosion resistance of bonded Nd-Fe-B magnets, and reduces the hygroscopic properties. The molecule of sodium silicateis rigid and keeps it original shape at high temperature environments. In addition, SS in composite binder improves the mobility of the magnetic powders during the pre-pressing process, which makes the magnetic powders attain a more regular structure. These two factors will increase the mechanical properties. Moreover, sodium silicate in the composite binder can also cover the surfaces protecting the magnetic powders from oxidation and corrosion. EP in composite binder can cover SS surface to reduce the water absorption of SS as epoxy is a hydrophobic material. The EDX analysis shows that the composite binder has accumulated in the gaps of the magnet powders, which not only improves heat resistance and corrosion resistance, but also increases the mechanical properties. Therefore, EP/SS composite binder endows bonded Nd-Fe-B magnets excellent comprehensive properties.     

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.     

(Nd,Pr,Ce)-Fe-B磁体的组织与磁学性能

为开发低成本烧结钕铁硼磁体,用30% Ce替代(Nd_0.75Pr_0.25)_32.69Fe_66.25B_1.06磁体中的Nd和Pr,研究了磁体在烧结及回火过程中的组织结构和磁学性能变化.结果表明,取向压坯在1030~1080℃烧结2 h后,随烧结温度升高,磁学性能下降,烧结温度为1030℃时综合磁学性能均最好.烧结态Ce替代磁体的综合磁学性能优于未替代磁体.一级回火后,相组成和晶粒尺寸基本不变,边界结构也未发生明显变化,磁体性能基本不变,或有少量下降.二级回火后,晶界明显改善,获得较清晰且平直的晶界,磁体矫顽力均得到大幅提高.Ce替代磁体的剩磁、矫顽力和磁能积均稍低于未替代磁体.      

压坯密度对烧结NdFeB磁体磁性能的影响

采用速凝片（SC）、氢破（HD）和气流磨（JM）工艺制备钕铁硼磁粉,研究了压坯密度、烧结温度对磁体取向度、微观结构和磁性能的影响。结果表明：选择合理的压坯密度（ρx=3．4g／cm3）可以使磁体在模压和液相烧结过程中保持较高的取向度,剩磁提高约2％。在低温度（1055℃）烧结时,可以获得较为理想的显微组织,主相晶粒细小...     

Effect of Copper and Titanium Addition on Microstructures and Magnetic Properties of Sintered Nd_(22) Fe_(71) B_7 Magnets

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Influence of Heat Treatment on Microstructures and Properties of Nd8Fe78B6Co4 Alloy

Melt-spun Nd8Fe78B6Co4 magnetic powders and their bonded magnets were prepared with the optimization of compositions and preparation techniques. The microstructure change of alloy NdFeB and the relation between microstructure and heat-treatment were studied. The heat-treatment temperature is 200～700 ℃. The as-cast structure of the alloy is typically amorphous. Different melt-spun speed and different heat treatment could result in different magnetic properties of NdFeB magnets. Magnetic properties of NdFeB increase with the addition of element Co. The magnetic properties of magnet alloy get the best when the melt-spun speed reaches 23～26 m·s-1, heat treatment temperature is 690 ℃ and time is 30 min.     

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.     

Study on Compound Effect of Bonded Magnets

The compound effect of Nd2Fe14B/Fe3B-Ferrite bonded magnets was studied.The result shows that the value ofβjHC obviously decreases with the ferrite content increasing.In addition, a functional relation between magnetic properties and ferrite content was clearly revealed by the physical relation in the magnetic powders.     

Enhanced magnetic properties in chemically inhomogeneous Nd-Dy-Fe-B sintered magnets by multi-main-phase process

Homogeneous substitution of Dy for Nd in the hard magnetic 2:14:1 phase can effectively enhance coercivity to ensure the high temperature operation,however,inevitably deteriorate remanence at expense.In this work,we performed a comparative investigation of the two magnets prepared by multimain-phase(co-sintering Nd_2 Fe_(14)B and(Nd,Dy)_2 Fe_(14)B powders) and single-main-phase(sintering(Nd,Dy)_2 Fe_(14)B powders) approaches.The comparative investigation reveals that at the same Dy substitution level(2.16 wt%),such chemically inhomogeneous multi-main-phase magnet possesses better roomtemperature magnetic properties as well as thermal stability than those of the single-main-phase one with homogenous Dy distribution in the matrix grains.Room-temperature magnetic properties H_(Cj)=1664 kA/m,B_r=1.33 T and(BH)_(max)=350.4 kJ/m~3 for the multi-main-phase magnet are all better than those for the single-main-phase magnet with H_(Cj)=1536 kA/m,B_r=1.29 T and(BH)_(max)=318.4 kj/m3.In addition,over the temperature range from 295 to 423 K,both the temperature coefficients of coercivity and remanence for the multi-main-phase magnet are also lower than that for the single-main-phase magnet.Such superior magnetic performance is attributed to the short-range magnetic interactions inside individual 2:14:1 phase grains and the long-range magnetostatic interactions between adjacent grains with inhomogeneous Dy distribution.Our work provides a feasible approach of enhancing coercivity and retaining energy product simultaneously in the Nd-Dy-Fe-B permanent magnets.     

烧结温度对Nd24.38Ce0.52Gd6.65Febal.TM1.76B0.95磁体组织与性能的影响

采用双合金法制备Nd24.38Ce0.52Gd6.65Febal.TM1.76B0.95（质量分数,%）永磁体,通过扫描电镜及能谱、AMT-4磁测试仪、电子万能力学试验机等手段研究烧结温度对磁体组织和性能的影响.结果表明：随烧结温度从1060℃升高到1100℃,在烧结温度为1080℃时,晶粒均匀且结合致密,富稀土相分布均匀,能获得较好的组织形态;富稀土相中稀土总含量从84.98%增加到98.04%,烧结过程中铈从主相显著扩散到富稀土相;磁体剩磁Br、矫顽力Hcj、磁能积（BH）max 先升后降,在1080℃烧结时获得较好的磁性能,分别为1.22 T、964 kA/m 和293 kJ/m3,同时磁体抗弯强度也达到最大值为257 MPa.