Microstructural investigation of Nd-rich phase in sintered Nd-Fe-B magnets through electron microscopy

The distribution, morphologies and structures of intergranular Nd-rich phase in sintered Nd-Fe-B magnets were studied through electron microscopy. Backscattered electron (BSE) imaging revealed that Nd-rich particles with various morphologies and sizes were randomly distributed at the grain boundaries and the triple junctions of the tetragonal Nd2Fe14B matrix. Through selected area electron diffraction (SAED) analysis under a systematic tilting condition, most intergranular Nd-rich phase particles, with sizes ranging from hundreds of nanometres to several micrometres, were identified as face-centred cubic (FCC) structure. Such particles possessed several approximate orientation relationships with their adjacent Nd2Fe14B matrix grains, such as (002) Nd2Fe14B//(200) FCC_Nd-rich [120] Nd2Fe14B//[001] FCC_Nd-rich , (002) Nd2Fe14B//( 220 ) FCC_Nd-rich [110] Nd2Fe14B//[112] FCC_Nd-rich , as well as (011) Nd2Fe14B//(131) FCC_Nd-rich [111] Nd2Fe14B//[114] FCC_Nd-rich , which could be attributed to minimising interfacial energy. The combination of highresolution electron microscopy with energy-dispersive X-ray spectroscopy revealed the internal inhomogeneous nature of Nd-rich phases. The large lattice distortion and nanoscale-ordered structures within a single Nd-rich grain were observed.     

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.     

添加不同钐含量的Sm2Fe17型合金及其氮化物的研究

通过采用粉末冶金法及密封氮化的方法，对添加不同钐含量的Sm2Fe17型合金及其氮化物的组织形貌、物相组成与结构及磁性能进行了研究。结果发现，多补偿添加25％钐可以使Sm2Fe17型合金退火态的α—Fe含量小于2％。Sm-Fe合金冶炼后的主相均表现为菱方Th2zn17型结构，但快冷时优先沿{300}和{220}面长大。氮化后Sm2Fe17晶格膨胀形成Sm2Fe17N，主相，而α—Fe的X射线特征峰未见明显移动。Sm14．2FeB58合金晶胞膨胀相对较小，而Sm12.8Fe87.2晶胞膨胀较大，在氮化20h时有最大△V／V=8．36％：氮化增加合金中的α—Fe含量。Sm14．2Fes5．8N，的剩磁最高为59．5Am^2／kg，S1l0．5Fe89.5Nx磁化强度最高值为193．6Am^2／kg，Sm12．8Fe87．2Nx合金的所有磁性能值基本分布在Sm14．2Fe85．8Nx和Sm10．5Fe89．5Nx的值之间。     

Influence of gadolinium on microstructure and magnetic properties of sintered NdGdFeB magnets

The effect of Gd content on microstructure and magnetic properties of sintered Nd33.03-xGdxFe65.65B1.32 (x=0-2) was studied in this paper to improve the thermal stability of NdFeB and to reduce the raw material cost. The results showed that better magnet performance could be obtained by adding Gd (0-1.5 wt.%) with partial substitution of Nd in Nd33.03-xGdxFe65.65B1.32. It was also found that the Nd33.03-xGdxFe65.65B1.32 magnets showed the best performance when Gd addition increased to 1.0 wt.%. The temperature coefficient Br (α) could be improved from -0.15%/oC to -0.063%/oC (maximum work temperature 120 oC) and the Curie temperature could be improved from 315 oC to 323 oC because the Gd2Fe14B had positive temperature coefficient Br (α) and higher Curie temperature than that of Nd2Fe14B. The coercivity could be improved from 10.2 to 11.48 kOe and the microstructure was close to ideal microstructure. The magnetic performance decreased sharply by adding Gd (above 2 wt.%) with partial substitution of Nd in Nd33.03-xGdxFe65.65B1.32 because the Gd element concen-trated in the grain boundaries.     

Microstructure and corrosion resistance of sintered NdFeB magnet modified by intergranular additions of MgO and ZnO

Microstructure and corrosion resistance of sintered Nd15Dy1.2Fe77Al0.8B6 and Nd22Fe71B7 magnets modified by intergranular addition of MgO and ZnO were investigated. Both the remanence and sintering density of the magnets increased slightly with intergranular additions of MgO and ZnO. There was a remarkable increase in coercivity of Nd22Fe71B7 after addition. Besides, the effects on magnetic properties and an improved corrosion resistance were observed. Compared with the native magnets without addition, corrosion potential of the magnets with MgO and ZnO additives was more positive and the current density in the anodic branch of the polarization curve was reduced. Corrosion resistance resulting from autoclave testing （2×10^5 Pa of steam pressure, 120 ℃） showed that the corrosion rate of NdFeB magnets reduced with the increase of additive amount. Microstructure observation revealed that MgO and ZnO additives were incorporated into the intergranular phases in the magnets. With the introduction of MgO and ZnO, more intergranular phase with high oxygen content was formed while keeping the volume fraction of all the intergranular phases almost unchanged, which may contribute to improved corrosion resistance. Furthermore, addition of MgO and ZnO refined the grain size of Nd22Fe71B7.     

高矫顽力2:17型SmCo稀土永磁的时效处理与磁性能的研究

利用X射线衍射仪、扫描电子显微镜、X射线电子能谱分析以及磁性测量的方法,研究了高矫顽力2:17型钐钴稀土永磁合金在等级时效过程中磁性能的变化与时效条件及显微组织结构的关系.合金一经时效就由单相固溶体分解为2:17相和1:5相,在随后降低温度的等级时效过程中,内禀矫顽力由398 kA/m提高到1 631.8 kA/m,Hci的提高可以认为是两相畴壁能差的变化引起的,另外时效中产生的晶界析出物对矫顽力的提高也起了一定的作用.     

Effect of cobalt substitution on magnetic properties and microstructure of nanocrystalline （NdDyTb）12.3（FeZrNbCu）81.7B6.0 ribbons

Effect of Co substitution and annealing treatment on the formation, magnetic properties and microstructure of (NdOyTb)12.3(FeZrNbCu)81.7CoxB6(x=0-15) ribbons prepared by rapid quenching and subsequent annealing was systematically investi-gated by means of differential scanning calorimeter (DSC), X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM) and vibrating sample magnetometer (VSM). Phase analysis revealed single-phase material. The remanence polarization Jr and maximum en-ergy product (BH)max increased with increasing x from 0 to 12 and then decreased for x=lS. The intrinsic coercivity Hci of (NdDyTb)12.3 (FeZrNbCU)81.7-xCoxB6 ribbons optimally processed decreased from 1308.7 kA/m for x=0 to 817.4 kA/m for x=15. Optimum magnetic properties with Jr=1.041 T, Hci=944.9 kA/m and (BH)max=155.1 kJ/m3 were achieved by annealing melt-spun ribbon (x=-12) at 675℃ for 10 min. There was no significant influence of Co substitution on microstructure.     

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.     

Effect of yttrium substitution on magnetic properties and service performances of Nd-Fe-B sintered magnets

We successfully fabricated partial Y substituted NdY-Fe-B magnets with nominal compositions of(Nd_1-xY_x)_13.80Fe_ba1Al_0.24Cu_0.1B_6.04(at%,x=0,0.1,0.2,0.3,0.4) by powder metallurgy process and the magnetic properties as well as service performances of the magnets were also systematically investigated.The phase constituents of the magnets have no obvious variation within the whole range of Y content,while the main phase grain...     

Influence of La-Co substitution on the structure and magnetic properties of low-temperature sintered M-type barium ferrites

La-Co substituted M-type barium ferrites (BaM) were prepared by traditional solid state method and sintered at low tem-perature (1173 K). X-ray diffraction (XRD), scanning electron microscopy (SEM) and...     

放电等离子烧结技术制备Sm2Fe17Nx烧结磁体的研究

采用放电等离子烧结技术制备了Sm2Fe17Nx烧结磁体,考查了压力、烧结温度和升温速率对烧结磁体性能的影响.结果表明:随压力的增加,磁体的致密度显著提高,但Sm2Fe17Nx分解成SmN、α-Fe和N2的程度加剧,造成磁体的矫顽力明显下降,在1GPa的高压下烧结时,超过200℃后磁体的矫顽力就下降很快,说明高压促进了Sm2Fe17Nx的低温分解;采用升温速率为450℃/min的快速烧结工艺,发现未能有效地抑制Sm2Fe17Nx的分解.     

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.     

粉末特性对Sm2(Co,Cu,Fe,Zr)17永磁材料及性能的影响

在粉末冶金工艺生产Sm2(Co,Cu,Fe,Zr)17的过程中,粉末特性对材料的性能存在较大影响.本研究对气流磨和滚动球磨两种工艺所制备的粉末进行比较,通过粒度分析及显微镜观察,研究了粉末的粒径与形状对材料性能的影响.分析结果表明,气流磨所制备的粉末平均粒径为4.53μm,尺寸分布范围较窄,粉末颗粒成近似球状,所得材料磁性能参数中Br,(BH)max优于滚动球磨.     

Influence of zirconium addition on microstructure, magnetic properties and thermal stability of nanocrystalline Nd12.3Fe81.7B6.0 alloy

Effect of Zr addition on microstructure, magnetic properties and thermal stability of Nd12.3Fe81.7B6.0 (x=0-3.0) ribbons melt-spun and annealed was investigated. Magnetic measurement using vibrating sample magnetometer (VSM) revealed that Zr addition was significantly effective in improving the magnetic properties at room temperature. The intrinsic coercivity Hci of the optimally processed rib-boris increased monotonically with increasing Zr content, from 751.7 kA/m for x=0 to 1005.3 kA/m for x=3.0. Unlike the coercivity, the re-manence polarization Jr increased first with Zr addition, from 0.898 T up to 1.041 T at x=1.5, and then decreased with further Zr addition.The maximum energy product (BH)max behaved similarly, increasing from 103.1 KJ/m3 to a maximum of 175.2 kJ/m3 at x=1.5. Microstruc-ture studies using atomic force microscopy (AFM) and transmission electron microscopy (TEM) had shown a significant microstructttre re-finement with Zr addition. The absolute values of temperature coefficients of induction and coercivity were significantly increased with in-creasing Zr content, indicating that Zr was detrimental to thermal stability of the melt-spun Nd2Fe14B-type material.     

2:17型SmCo永磁材料的研究进展与展望

2:17型SmCo永磁体自1977年问世以来,其研究得到很大发展,性能不断提高.因其具有优异的磁性能,已在微波通讯技术、航空航天、国防工业、交通运输业等领域广泛应用.因2:17型SmCo永磁体具有较高的居里温度和较高的磁能积,而成为永磁材料的首选材料.作者介绍了2:17型SmCo永磁的发展过程、磁体的磁性能、制备工艺、应用情况及其发展趋势.     

Transport properties of Zintl phase Yb1-xCaxCd2Sb2 at low temperature

We investigated the transport properties of isoelectronic substitution of Yb by Ca for Zintl phase YbCd2Sb2 below 300 K.The p-type Yb1-xCaxCd2Sb2(0.2≤x≤0.8) samples were synthesized via a solid-state reaction followed by suitable cooling,annealing,grinding,and spark plasma sintering(SPS) densification processes.For samples with x=0.2,0.4,0.5,0.6,0.8,the electrical conductivity,Seebeck coefficient,thermal conductivity,heat capacity and Hall effect measurements were carried out in the temperature range from 1...     

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.     

Effect of chromium on magnetic properties and corrosion resistance of LaFe11.5Si1.5 compound

Effects of Cr addition on magnetic and corrosion properties of LaFe11.5-xCrxSi1.5 (x=0.1, 0.3, 0.4) magnetic refrigerants were investigated. It was found that the addition of Cr slightly decreased the magnetic entropy change, but it was effective in increasing corrosion resistance of La-Fe-Si compounds within the composition range examined. Corrosion measurements showed that corrosion current density of these La-Fe-Si compounds in distilled water decreased from 2.6×10-6 to 8.7×10-7 A/cm2, with x increasing from 0 to 0.3, while magnetic entropy change in LaFe11.5-xCrxSi1.5 compounds did not change significantly (-ΔSmax was 18.0, 17.0, 13.6, 11.1 J/(kg·K)) under 2 T for x=0, 0.1, 0.3, 0.4, respectively). Surface optical microstructures of compounds after corroded showed that corrosion took place at grains and grain boundaries simultaneously and surface concentration of corroded points on LaFe11.5-xCrxSi1.5 (x=0.1, 0.3, 0.4) compounds reduced obviously.