爆炸压结Nd-Fe-B永磁体微观结构

利用透射电镜、X射线衍射仪、X射线能谱仪，对爆炸压结Nd-Fe-B永磁合金进行微观组织结构的观察和分析。结果表明：爆炸压结Nd-Fe-B的组织主要由基体Nd2Fe14B相、富O相和富Nd相组成；基体相是硬磁相，四方晶体结构，其晶格常数为a=0．88nm和c=1．22nm；富O相形貌呈三角状或层状，分布在3个晶粒交隅处和两个晶粒交界处，其晶体结构均为面心立方（fcc），点阵常数a=0.559nm；富Nd相呈不同块状形貌，镶嵌存基体内或晶界上，其晶体结构为密排六方（hcp），晶格常数a=0．395nm和c=0.628nm：在富O相中O，Nd和Fe的含量（原子分数，下同）分别为45％～60％，20％～40％和10％～12％，块状富Nd相中则为80％～85％Nd和10％～l5％O，同时还发现晶界相中分布着少量的位错。     

烧结NdFeB磁体热压变形后富Nd相的显微组织

采用热压变形法对NdFeB磁体晶间富Nd相的显微组织进行了研究,实验结果表明,NdFeB磁体经真空热压变形后,富Nd相不再平均地分布在磁体晶间,而是聚集成团块状或从磁体边缘渗出,显微组织分析表明,富Nd相主要是由α-Dd和Nd2Fe17两相组成,与Nd-Fe合金的共晶组织成分接近,对于晶间添加Al元素的磁体,Al溶入晶间形成Nd2Fe15Al2相弥散地分布在晶界上,这有益于磁体矫顽力的提高;对于晶间添加Cu元素的磁体,晶间没有发现有新相产生。     

富钕相对烧结NdFeB磁体耐腐蚀性的影响

研究了Nd2Fe14B单晶、传统烧结NdFeB磁体和放电等离子烧结（简称SPS）NdFeB磁体在电解液溶液中的电化学特性。采用扫描电子显微镜和电子能谱分析了磁体的微观组织成分。结果表明在3．5％NaCI溶液的极化曲线中，Nd2Fe14B单晶具有最高的电化学腐蚀电位，放电等离子烧结NdFeB磁体的腐蚀电位高于传统烧结NdFeB磁体。与传统烧结NdFeB磁体相比，放电等离子烧结NdFeB磁体富Nd相具有独特的分布形态，主相Nd2Fe14B晶粒细小、均匀，富钕相在主相晶粒边界上分布较少，主要集中在三角晶界处。这种组织结构有效地抑制了磁体沿富钕相发生晶间腐蚀的过程，磁体因此具有良好的耐腐蚀性能。此外，从不同稀土含量的烧结NdFeB磁体的高压加速实验中可以看出磁体的腐蚀速度随稀土含量的增加而增大。以上结果表明富Nd相的化学特性及其分布状态和含量是决定合金耐蚀性能的关键，它在合金中以网络状分布在主相晶粒边界上，并决定了烧结NdFeB易于发生选择性晶间腐蚀，从而导致耐蚀性差。     

Effect of Annealing on the Magnetism of the Sintered NdFeB Magnet

This paper deals with the effect of annealing on the magnetism of the sintered NdFeB magnet with a composition of Nd30B5.1Dy1.2Al0.6Nb0.7Fe62.4. Microstructural investigations of the grain size and grain boundaries with SEM were carried out. Microstructural investigations showed the presence of some Nd-rich phase in grain boundaries and main phase.The results of magnetic properties analysis shows that this non-magnetic Nd-rich phase, produced in annealing process,can increase or decrease the magnetism of the sintered NdFeB-type permanent magnet. Appropriate amount of Nd-rich phase will strengthen the pinning field and elevated the coercive force of magnet, but too many these non-magnetism phases in Nd2Fe14B main phase will decrease it. When the sintered NdFeB magnet was annealed at 3Pa and 492℃ for an hour the coercive force would raise from 915.6kA/m to l164.SkA/m, and the (BH)max from 277.7kJ/m to 349.5kJ/m. However, annealing at a non-optimized temperature at 542℃, microstructure changes in some main phase will leading the decrease of properties.     

机械力驱动下Nd16Fe76B8合金氢化-歧化反应机理研究

对机械力驱动下Nd16Fe76B8合金的氢化-歧化反应机理进行了研究。通过测量球磨过程中合金的吸氢量变化,揭示了其氢化-歧化反应动力学特征。采用X射线衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)等方法,研究了球磨过程中合金的组织演变。结果表明:在球磨的最初阶段,合金只发生氢化反应,生成NdH2.7与Nd2Fe14BHy相,此后随着球磨时间的延长,氢化态合金粉末在机械球磨的作用下被激活至高能状态,并逐渐发生歧化,最终得到晶粒尺寸约10nm的NdH2.7、Fe2B、α-Fe的纳米歧化组织。     

Fabrication of ultrafine Nd-Fe-B powder by a modified reduction-diffusion process

In order to obtain ultrafine Nd-Fe-B powder, a spray-dried precursor was treated by reduction-diffusion (R/D) process.And, unlike the conventional R/D process, calcium reduction that is a crucial step for the formation of Nd2Fe14B was performed without conglomerating the precursor with Ca powder.By adopting this modified process, it is possible to synthesize the hard magnetic Nd2Fe14B at the reaction temperature as low as 850 ℃.The average size of Nd2Fe14B particles that are uniformly distributed in the optimally treated powder was ＜ ＜1 μm.Most Nd2Fe14B particles were enclosed with thin layers of Nd-rich phase.Typical magnetic properties of such powder without eliminating impurity CaO were iHc=～5.9 kOe, Br=～5.5 kG, and (BH)max=～6 MGOe.     

NdFeB磁体组成相的电化学腐蚀行为

研究了电解质溶液中，NdFeB磁体3个组成相(Nd2Fe 14B、Nd-rich和Nd1.1Fe4B4)的腐蚀电位、极化特性等电化学行为.结果表 明：3个组成相在不同的腐蚀介质中表现出不同的腐蚀规律，组成相之间的电偶电池效应加 速了NdFeB磁体的“相选择性腐蚀”过程.     

THE EFFECT OF Mo ADDITION ON COERCIVITY OF NdFeB SINTERED MAGNET PREPARED BY BLENDING METHOD

Alloy modification, accompanying with proper heat treatment, is commonly used to improve the thermal stability of NdFeB magnet. Traditional alloy modification is performed through melting process with alloy elements to form the multi-alloy. In doing so, these alloy elements not only are introduced into the inter-ranular boundaries, but partly into the main phase, thus decreasing to some extent the magnetism of the main phase. In this paper, the blending method is used to prepare the Nd22Fe71B7/Mo sintered magnet, and its magnetic properties and microstractures are investigated. The results show that by adding 1.5% （mass fraction） Mo, the intrinsic coercivity 24, of the magnet reaches the maximum value of 1719.36KA/m, while continually increasing the amount of Mo has a less effect on iHc Microstructures analysis indicates that Mo-free Nd-Fe-B magnet has not uniform grains in size, while that with Mo element has uniform grains in size and smooth grain boundaries. Experiments show that after the NdFeB magnet is sintered at 1273K and annealed at 873K, the added Mo element could prevent the equilibrium transformation between the main phase and Nd-rich phase, thus resulting in the precipitation of fine second main phase （Nd2Fe14-xMoxB） from the main phase boundaries, preventing the nucleation and expansion of anti-magnetic domain, and enhancing the coercivity.     

Investigation of the coercivity mechanism for Nd-Fe-B based magnets prepared by a new technique of strip casting

The coercivity mechanism of Nd-Fe-B based magnets prepared by a new technique of strip casting was investigated. Different from the traditional magnets, α-Fe phases are difficult to be found in Nd-Fe-B magnets prepared by strip casting. Meanwhile, the rich-Nd phases occur not only near the grain boundaries of main phases, but also within the main-phase grains. Investigation on the magnetizing field dependence of the eoercivity for the (Nd0.935Dy0.065）14.5Fe79.4B6.1magnet and the temperature dependence of the coercivity for the Nd14.5Fe79.4B6.1magnet have been done. Results show that coercivities for strip casting magnets are controlled by the nucleation mechanism.     

Nd_(90)Al_(10)晶界调控对晶界扩散磁体磁性能和微观结构的影响EI北大核心CSCD

采用添加Nd_(90)Al_(10)低熔点合金调控制备了扩散用烧结Nd_2Fe_(14)B磁体,并采用Tb晶界扩散制备了相应的扩散磁体,分析了扩散磁体的晶界结构和成分对磁体矫顽力的影响。结果表明,添加质量分数为0.5%的Nd_(90)Al_(10)合金调控后,晶界扩散(GBD)后磁体的矫顽力提高到1439 kA/m,相对于未晶界调控的扩散磁体增加了530 kA/m。添加Nd_(90)Al_(10)低熔点合金不会影响GBD前磁体的Curie温度,但降低了磁体的低温相变温度。GBD后磁体Tb取代晶格中的Nd引起Nd_2Fe_(14)B相的晶格常数减小,从而使XRD谱中衍射峰位右移。经Nd_(90)Al_(10)调控后的扩散磁体表面处的主相晶粒的富Tb壳清晰可见。从距离磁体表面20μm增加到100μm时,富Tb壳层仍清晰可见。当深度继续增加到500μm时,经Nd_(90)Al_(10)调控后的扩散磁体晶粒周围都有连续晶界相。经晶界调控的扩散磁体可见衬度明显的富Tb壳层,形成了非晶的富Nd相,增强了两两主相晶粒间的去磁耦合能力。Nd在富Nd相中心区域出现峰值,更多的富Nd相在晶界扩散过程中作为Tb向磁体内扩散的通道,Tb原子在富Nd相的浓度高达约35%,其扩散深度和使用效率明显提升。     

Grain boundary microstructure in DyF3-diffusion processed Nd-Fe-B sintered magnets

The effect of post-sinter tempering on the DyF₃-diffusion processed Nd-Fe-B was investigated using two kinds of starting magnets. The increase of coercivity after diffusion process using as-sintered magnet was higher than that using two-stage tempered magnet. The grain boundary phase of the tempered magnet became discontinuous upon further annealing at the temperature of diffusion process. This clearly indicates that a continuous grain boundary phase is helpful to the DyF₃-diffusion process. When sufficiently diffused, there is no enrichment of Dy in the grain boundary phase. The excess Nd as a result of Dy substitution in the Nd₂Fe₁₄B matrix phase forms Nd-O phase at grain boundary and on the surface of the magnet. The increase of coercivity can be related to the (Nd,Dy)₂Fe₁₄B grains as well as to the improved decoupling by the grain boundary phase.     

两种方法制备纳米晶复相Nd2Fe14B/α-Fe永磁体实验研究

将机械球磨后制备的Nd2Fe14B非晶粉末和α-Fe纳米晶粉末分别采用2种方法制备纳米复相Nd2Fe14B/α-Fe永磁体。第1种方法是直接将其冷压制坯、真空包套和热挤压制备永磁体。第2种方法是先将Nd2Fe14B晶化,然后冷压制坯、真空包套和热挤压制备永磁体。利用TEM、VSM等分析手段对比研究了2种方法制备永磁体的相对密度、微观组织以及磁性能。结果表明:在相同的工艺参数下,第1种方法制备永磁体不仅可以减少工序,而且其制备的永磁体综合性能均优于第2种方法,其制备永磁体的相对密度为98.24%;Nd2Fe14B和α-Fe的晶粒尺寸分别为60和80nm;磁性能达到:Br=0.98T,Hci=305.6kA/m,和(BH)m=89.8kJ/m3。     

高矫顽力的低钕Nd9(FeCoZrAl)85B6纳米晶合金的制备

采用单辊快淬工艺制备了一种低钕含量Ｎｄ９（ＦｅＣｏＺｒＡｌ）８５Ｂ６纳米晶合金,研究了快淬工艺与热处理工艺对该合金纳米晶的形成及磁性的影响。结果表明快淬速度和热处理温度都明显地影响低钕含量Ｎｄ９（ＦｅＣｏＺｒＡｌ）８５Ｂ６纳米晶的形成及其磁性（内禀矫顽力ｊＨｃ,矫顽力ｂＨｃ,剩磁Ｂｒ和最大磁能积（ＢＨ）ｍ）。快淬速度２３ｍ／ｓ制备的非晶态合金,在６８５℃处理３０ｍｉｎ,可获得最佳的磁性,其粘结磁体的密度为６．０１ｇ／ｃｍ３时,Ｂｒ＝６５５ｍＴ,ｊＨｃ＝６３９．２ｋＡ／ｍ,ｂＨｃ＝３８１．６ｋＡ／ｍ,（ＢＨ）ｍ＝６５．６８ｋＪ／ｍ３。     

HDDR各向异性NdFeB矫顽力机理的研究

研究了HDDR各向异性NdFeB永磁材料的矫顽力机理。通过对材料磁化过程的研究以及对其显微组织结构的观察分析，发现其矫顽力机制起源于畴壁挣脱主相Nd2Fe14B晶粒边界以及晶粒团边界富钕相的钉扎机制，其中富钕相对材料畴壁的钉扎是决定其矫顽力的关键因素。通过理论计算，其结果与材料实际的矫顽力十分接近。此外，还进行了验证性实验并提出了改善材料矫顽力的途径。     

High-coercivity Nd–Fe–B thick films without heavy rare earth additions

The magnetic properties and microstructures of two Nd–Fe–B thick films with different Nd contents have been studied. The films were deposited in the amorphous state and were crystallized by post-deposition annealing. Both films show a strong 〈0 0 1〉 fibre texture out-of-plane. The film with the higher Nd content has a large room temperature coercivity of 2.7 T, while the one with the lower Nd content has a room temperature coercivity of only 0.7 T. The difference in coercivity may be explained by the fact that the film with the higher Nd content exhibits a continuous Nd-rich grain boundary phase, giving better isolation of the Nd₂Fe₁₄B grains with respect to magnetic exchange interactions. The extrusion of Nd-rich liquid to the top surface of the film with high Nd content during post-deposition annealing led to the formation of ripples in the Ta capping layer, indicating that the films are under compressive stress. This stress-induced flow of the Nd-rich material up through the film explains the excellent distribution of the Nd-rich grain boundary phase. Atom probe tomography has revealed the presence of Cu in the Nd-rich grain boundary phase, explaining the formation of the liquid phase at the relatively low temperature of 550 °C due to the eutectic reaction of Nd and Cu.     

烧结NdFeB磁体相的继承性研究

设计成分为Nd32.5B1.04Febal(质量分数,%),经过熔炼,制粉,成型,烧结后制备了烧结NdFeB磁体,对样品的铸锭,烧结态样品以及高温回火态样品,低温回火态样品的微观组织采用SEM进行了仔细地分析。结果显示,烧结NdFeB磁体的相具有"继承性",在熔炼中产生的α-Fe相会被烧结回火后的磁体继承下去,而烧结中形成的Nd2Fe14B相和B-rich相在回火后数量和形态基本上变化不大,Nd-rich相虽然数量变化也不大,但是在高温回火中熔化流动,均匀分布在主相Nd2Fe14B周围,把主相Nd2Fe14B一个个分隔开来,在低温回火中,这种流动会延续,相的形态会得到巩固,使得磁体最终获得良好的综合磁性能。     

添加Nb对Nd—Fe—B磁体温度稳定性的影响

对Nd15.15Fe78.11-xNbxB6.74(x=0,0.21,0.42,0.72,1.08,1.44)永磁体的温度特性和显微组织及两者之间的关系进行了研究，结果表明：Nb可以显著降低磁体的磙这不可逆损失，但对磁体磁通可逆部分几乎没有影响，Nb对Nd-Fe-B磁体中的作用是使晶粒均匀化，规则化，导致晶粒表面层厚度r0大幅度变薄，晶粒表面的最小形核场H11和Bloch壁的挣脱钉扎场HN增大，因而使磁体的不可逆损失降低，温度稳定性和使用温度提高。     

Effect of post-sinter annealing on the coercivity and microstructure of Nd–Fe–B permanent magnets

To understand the mechanism of the increase in coercivity caused by post-sinter annealing of Nd–Fe–B-based magnets, we have investigated the microstructures of commercial sintered magnets by high-resolution scanning electron microscopy, transmission electron microscopy and atom probe tomography. Continuous thin layers of a Nd-rich amorphous phase were found along the grain boundaries in the post-sinter annealed sample, the chemical composition of which was determined to be Nd₃₀Fe₄₅Cu_24.1B_0.9. A fine Cu-enriched shell was also confirmed in the Nd-rich phase grain, suggesting the Nd₂Fe₁₄B grains are completely enveloped by the Cu- and Nd-enriched layers. Furthermore, a lamellar microstructure of the Cu-enriched phase was confirmed in some Nd-rich phase grains. The mechanism of the coercivity increase caused by post-sinter annealing is discussed based on these characterization results.     

High-coercivity ultrafine-grained anisotropic Nd–Fe–B magnets processed by hot deformation and the Nd–Cu grain boundary diffusion process

The grain boundary diffusion process using an Nd₇₀Cu₃₀ eutectic alloy has been applied to hot-deformed anisotropic Nd–Fe–B magnets, resulting in a substantial enhancement of coercivity, from 1.5 T to 2.3 T, at the expense of remanence. Scanning electron microscopy showed that the areal fraction of an Nd-rich intergranular phase increased from 10% to 37%. The intergranular phase of the hot-deformed magnet initially contained ～55 at.% ferromagnetic element, while it diminished to an undetectable level after the process. Microscale eutectic solidification of Nd/NdCu as well as a fine lamellae structure of Nd₇₀(Co,Cu)₃₀/Nd were observed in the intergranular phase. Micromagnetic simulations indicated that the reduction of the magnetization in the intergranular phases leads to the enhancement of coercivity in agreement with the experimental observation.     

EFFECT OF Nb ADDITION ON MICROSTRUCTURE OF(Nd,Dy)-(Fe,Co)-B MAGNETS

An addition of Nb up to 2 at.-% into(Nd,Dy)-(Fe,Co)-B alloy causes the formation ofdendrite Fe_2Nb and the precipitates in hard magnetic grains.Both increases withincreasing Nb content.During sintering,part of Fe_2Nb dissolves within the 2:14:1 grains,and the Fe_2Nb along grain boundaries hinders the growth of 2:14:1 grains.During an-nealing,the dissolved Nb in(?)-phase precipitates out,and this nearby the grain boundarydiffuses into Nd-rich phase to form new granular Fe_2Nb and to increase the Nb contentin Nd-rich phase,this results in a precipitate-free zone in the(?)-grain near Nd-rich phase.