Effect of Al and Al/Mo addition on microstructure and magnetic properties of sintered Nd22Fe71B7 magnets

1　ＩＮＴＲＯＤＵＣＴＩＯＮＩｔｉｓｗｅｌｌｋｎｏｗｎｔｈａｔｔｈｅｉｎｔｅｒｇｒａｎｕｌａｒｍｉ ｃｒｏｓｔｒｕｃｔｕｒｅｏｆｓｉｎｔｅｒｅｄＮｄ Ｆｅ Ｂｍａｇｎｅｔｓｐｌａｙｓａｋｅｙｒｏｌｅｉｎｄｅｖｅｌｏｐｉｎｇｔｈｅｉｒｃｏｅｒｃｉｖｉｔｙ[1,2 ].Ｅａｒｌｉｅｒｓｔｕｄｉｅｓｓｈｏｗｅｄｔｈａｔｔｈｅｉｎｔｅｒｇｒａｎｕｌａｒｍｉｃｒｏｓｔｒｕｃｔｕｒｅｉｓｃｏｍ ｐｏｓｅｄｏｆａＮｄ ｒｉｃｈｐｈａｓｅａｎｄａｓｍａｌｌａｍｏｕｎｔｏｆＢ ｒｉｃｈｐｈａｓｅ[3].Ｉｔｈａｓｂｅｅｎｓｈｏｗｎ…     

回火处理对烧结钕铁硼永磁材料组织和磁性能的影响

探讨了回火处理对烧结Nd-Fe-B系合金显微组织和磁性能的影响.研究表明回火处理后,磁体的显微组织得到明显的改善,主相体积分数增加,晶界变得清晰,晶粒尺寸趋向均匀;颗粒状富Nd相减少,富Nd相沿晶界均匀分布,成分趋于共晶富Nd相的成分;磁体的剩磁、矫顽力和最大磁能积都得到提高,最大磁能积普遍提高20～30 kJ/m3.     

烧结NdFeB永磁体的腐蚀行为研究

通过静态腐蚀实验,研究了烧结钕铁硼磁体在3.5 wt.% NaCl溶液中浸泡不同时间段的腐蚀特征。采用扫描电镜、拉曼光谱分析各个阶段的腐蚀形貌和腐蚀产物组成,通过动电位极化曲线、电化学阻抗谱研究不同腐蚀阶段磁体表面结构的变化及腐蚀机理,采用等效电路模型模拟各阶段的腐蚀行为。研究结果表明,烧结NdFeB磁体在3.5 wt.% NaCl溶液中依次发生点蚀、选择性晶间腐蚀、全面腐蚀行为,形成的腐蚀产物层结构疏松,只能产生短时减缓腐蚀速率的效果,而富钕相优先溶解会造成主相颗粒脱落,导致磁体粉化、破坏。腐蚀产物类型随腐蚀时间延长而有所变化,主要为铁和钕的氧化物或氢氧化物。     

优化边界结构改善烧结Nd-Fe-B永磁材料的力学性能

在富稀土辅合金中添加Co,Nb,Ti,Ga,Al等元素,用双合金工艺制备一系列不同辅合金含量的烧结Nd-Fe-B磁体,对力学性能进行系统研究。结果表明,在主合金(NdDyTb)12.69(FeCoNb)84.01B6.00的基础上添加3.0wt%的(NdDyTb)25(FeCoNbTiGaAl)68B7富稀土辅合金,其抗弯强度从316MPa提高到344MPa,抗弯强度的改善来自于边界结构的改善以及一些新相的生成。当辅合金含量达到8wt%,合金的强度又下降为321MPa。还研究了热处理工艺对Nd-Fe-B永磁材料力学性能的影响,含3.0wt%辅合金的磁体抗弯强度由烧结态的291MPa提高到最佳回火态的344MPa,又下降为非最佳回火态的304MPa。     

Corrosion protection of sintered NdFeB magnets by CAPVD Ti2N coating

Sintered NdFeB magnets have poor corrosion resistance and are readily susceptible to corrosion under different environmental conditions. Cathodic arc physical vapour deposited (CAPVD) titanium nitride coating for sintered NdFeB permanent magnets has been investigated in this paper. Tafel extrapolation was employed to study the corrosion behaviour in 3.5% NaCl solution at ambient temperature. The adhesive strength of the coating was estimated with the help of the scratch test. The surface chemistry and coating morphologies were studied with scanning electron microscope (SEM). X-Ray diffraction (XRD) was used for qualitative phase analyses of coatings and substrate. The properties of CAPVD titanium nitride coating were compared with electrodeposited multilayer nickel–copper–nickel coating. It was figured out that the CAPVD titanium nitride coating had better adhesion strength and shifted the free corrosion potential (FCP) of the system towards positive potential, providing protection to the NdFeB substrate. However, the corrosion rate of CAPVD titanium nitride coating was more than the electrodeposited multilayer nickel–copper–nickel coating. The magnetic properties remained comparable.     

Temperature stability and microstructure of ultra-high intrinsic coercivity Nd-Fe-B magnets

The variations of intrinsic coercivity and remanence of sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity were investigated. The results showed that the intrinsic coercivity and remanence declined simultaneously with increasing temperature, but the squareness of the magnets has hardly been changed. The temperature coefficients of remanence （α） and coercivity （β） for the magnets were calculated by two different methods, and the variations of the temperature coefficients and the microstructure of sintered Nd-Fe-B magnets were analyzed. The temperature coefficients of remanence （α） and coercivity （β） for the sintered magnets are very small, and the existence of fine microstructure is necessary to obtain sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity.     

Microstructure and magnetic properties of Nd-Fe-B sintered magnets with P addition

In this paper,the effects of P doping on magnetic properties and microstructure were studied in Nd-Fe-B sintered magnets.With P doping,the grain size gets refined and the distribution of the main phase is optimized due to the reduction of the liquidus temperature.The liquidus temperature for the 0.05 wt% P-doped magnets is 1022 K,while that for the P-free magnets is 1038 K.As P content increases,the liquidus temperature significantly decreases.Clear and continuous grain boundary phases are formed in the P-containing magnets with smaller grain size.The optimized microstructure with average grain size of 8.43 μm is obtained in the 0.05 wt% P-doped magnets,which is approximately 0.69 μm smaller than that of P-free sintered magnets(9.12μm).Though P is usually thought to be an impurity element,it might be beneficial in Nd-Fe-B sintered magnets with proper addition.The coercivity of the0.05 wt% P-doped magnets could be increased to1283 kA·m~(-1),with slight changes of the remanence and the maximum magnetic energy product.NdP04 phases in the grain boundary are of hexagonal structure,while those at the triple junctions have monoclinic structure.Activated sintering is achieved by doping proper P element in the Nd-FeB sintered magnets.     

Statistical model of magnetization reversal in Nd-Fe-B sintered magnets

Statistical model of magnetization reversal was used to simulate the magnetization reversal behavior in the sintered Nd-Fe-B magnets with double grain-size distributions due to the abnormal grain growth (AGG). The magnetic properties and mechanical properties due to the formation of AGG grains in Nd-Fe-B sintered magnets were tested. The results show that the magnetic properties, especially the rectangularity were severely deteriorated after the formation of the AGG grains and a step was shown on the demagnetization curve, and the occurrence of AGG mayaccount for the poor rectangularity and existence of the step on demagnetization curve according to the statistical model of magnetization reversal. The fracture toughness and bending strength are lowered because of the stress concentration in the AGG grains. The SEM images show that the formation of AGG grains is caused by the solid sintering due to the absence of RE-rich phase. Statistical model of magnetization reversal can qualitative by explain the dependence of the magnetization reversal behavior on the grain size in the Nd-Fe-B sintered magnets.     

烧结(Nd,Tb)-Fe-B磁体的元素扩散、反磁化和矫顽力

采用双合金法将两种粉末混合制备烧结永磁体可提高磁体磁性能;但在烧结过程中两种粉末之间存在元素扩散,元素扩散对磁性能的影响程度需要进一步研究。本文将Nd13Fe81B6和TbHx粉末混合制备烧结磁体,Nd13Fe81B6磁体矫顽力为4.5 kOe。当TbHx混合量为3 wt.%,烧结磁体的矫顽力增加至20.0 kOe。通过热激活研究认为,磁畴壁的形核是反磁化需要经过的过程。由于热力学的原因Tb元素更容易扩散进入Nd2Fe14B主相而不是富集在晶间富稀土相。Tb元素进入主相替代Nd可形成具有更高各向异性场的(Nd,Tb)-Fe-B表层,在反磁化过程中晶粒表层磁畴壁的形核场会增加,因此矫顽力增加程度显著。但是,TbHx混合量超过5 wt.%,矫顽力增加幅度降低。对于TbHx混合量7 wt.%的磁体,元素分布显示在主相晶粒内部贫Tb区域明显增少,证实在烧结过程中更多Tb原子从晶粒表层扩散入晶粒内部,这样晶粒表层反磁化形核场的提高程度会减弱,因而磁体矫顽力增加幅度降低。本研究说明要提高双合金Nd-Fe-B磁体磁性能需进一步控制元素扩散并优化磁体的元素分布。     

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。     

氧含量对烧结钕铁硼磁体Dy晶界扩散的影响研究

本文主要研究了烧结钕铁硼磁体中氧含量变化对Dy晶界扩散后的Dy含量及矫顽力增加量的影响。选取多种高、低氧磁体进行Dy扩散处理后比较发现,低氧磁体的Dy扩散量和矫顽力提高量均明显高于高氧磁体。对9个0wt.%Dy的不同氧含量样品进行扩散再次确认,氧含量减少有利于Dy扩散量、矫顽力的提高。各样品成分梯度结果显示,低氧磁体的Dy扩散量由表及里全面高于高氧磁体,内外浓度梯度也小于后者。电子探针表征结果表明,低氧磁体Dy扩散后晶界处Dy富集条纹更明显、连续,完整包裹各个主相晶粒。这种结构优化也使低氧磁体各向异性场提高幅度大于高氧磁体。磁体中氧含量降低使富钕相在主相周边均匀连续分布,为后续进入磁体内部的Dy元素提供连续的扩散通道,从而使磁体的Dy扩散量和矫顽力提高量进一步提高。     

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.     

Effects of oxygen and carbon on the magnetic properties and microstructure of Sm2Co17 permanent magnets

The research on the sintered Sm2Co17 permanent magnets prepared by metal injection molding is still at the exploratory stage. Carbon and oxygen are two key factors that influence the magnetic properties. In this article, the effects of oxygen and carbon on the properties and microstructure of the magnets have been studied. The results indicate that oxygen consumes the effective Sm content of the magnets and forms Sm2O3-the non-magnetism phase, which result in the deterioration of the magnetic properties. Besides, the magnetic properties decrease in evidence with increasing carbon content. The main factor that affects the magnetic properties is the deterioration of the microstructure of the magnets. The Sm（Co, Cu）5 phase decreases, whereas the cell size increases with the increase of the carbon content. When the carbon content is above 0.43 wt.%, the Sm（Co, Cu）5 phase is not enough to form a uniform cellular microstructure. Thus the magnetic properties disappear. ZrC is detected in the magnets by XRD when the carbon content is above 0.21 wt.%. ZrC also reduces the properties of the magnets.     

Cu/Ti复合添加对Nd2Fe14B/α-Fe纳米双相磁体磁性能和相分解的影响

用熔体快淬法制备了高性能纳米双相耦合Nd2Fe14B/α-Fe磁体，研究了Cu/Ti复合添加对Nd2Fe14B/α-Fe纳米双相磁体磁性能和相分解的影响，实验结果表明，Cu和Ti复合添加可提高快淬带的晶化温度，并且改变α－Fe相析出方式，α－Fe直接从TbCu7结构的亚稳相分解中析出，而不是从非晶相中析出，这有利于形成α－Fe相晶粒细小且均匀分布的微结构，其最优磁性能为Hc=384kA/m(4.8kOe),σ＝110Am^2/kg(110emu/g),(BH)max=120kJ/m^3(15MGOe)。     

烧结钕铁硼(Al+Cu)含量对晶界扩散的影响

本研究对(Al+Cu)含量分别为0.25%的钕铁硼基体和0.5%基体进行Dy晶界扩散,并分析了矫顽力、Dy含量分布和微观结构。通过比较两种磁体的成分、性能发现,在Dy增加量基本相同的情况下,高(Al+Cu)磁体扩散后的矫顽力提高量相较于低(Al+Cu)磁体高37kA/m~43kA/m。进一步进行成分、矫顽力的梯度分析发现,基体的(Al+Cu)含量变化并没有改变扩散后磁体内部Dy元素随扩散深度的浓度分布,但是矫顽力梯度分析结果显示高(Al+Cu)的各片层矫顽力提升量均比低(Al+Cu)片层高40 kA/m~80 kA/m。后续的EPMA的Dy面分布图显示,高(Al+Cu)基体扩散后Dy在晶界处富集条纹更清晰、连续,而TEM的EDX分析结果也显示高(Al+Cu)样品中晶界附近Dy含量更高。(Al+Cu)含量的提高,使得晶界相的流动性增强,Dy更加连续包裹主相晶粒,使得Dy增加量相同的情况下进一步提升矫顽力。     

Magnetic properties and thermal stability of anisotropic bonded Nd-Fe-B magnets by warm compaction

Anisotropic bonded magnets were prepared by warm compaction using anisotropic Nd-Fe-B powder. The forming process, magnetic properties, and temperature stability were studied. The results indicate that the optimal temperature of the process, which was decided by the viscosity of the binders, was 110℃. With increasing pressure, the density of the magnets increased. When the pressure was above 700 MPa, the powder particles were destroyed and the magnetic properties decreased. The magnetic properties of the anisotropic bonded magnets were as follows: remanence Br = 0.98 T, intrinsic coercivity iHc=1361 kA/m, and maximum energy product BHmax = 166 kJ/m3. The magnets had excellent thermal stability because of the high coercivity and good squareness of demagnetization curves. The flux density of the magnets was 35% higher than that of isotropic bonded Nd-Fe-B magnets at 120℃ for 1000 h. The flux density of the bonded magnets showed little change with regard to temperature.     

纳米双相Nd2Fe14B/α-Fe磁体的微结构和交换耦合作用

用熔体快淬法制备了高性能纳米双相耦合Nd2 Fe14 B/α Fe磁体 ,研究了快淬速率对其微结构和交换耦合作用的影响。实验结果表明 ,控制快淬速率在 12m/s时 ,可直接得到显微组织均匀 ,α Fe相粒子细小且均匀分布的纳米双相耦合Nd2 Fe14 B/α Fe磁体。低温退火消除由快速凝固带来的成分不均匀性后 ,强烈的铁磁交换耦合作用导致其最高磁性能为 :iHc=432 .2kA/m ,Jr=1.0 8T ,(BH) max=115kJ/m3 。快淬速率提高 ,非晶相体积分数增加 ,在高温晶化热处理时软硬磁相析出不均匀 ,个别α Fe相粒子奇异长大 ,尺寸达到 10 0nm左右 ,这不利于软硬磁相间的交换耦合作用 ,有损磁性能。     

Structure and magnetic properties ofhigh-performanced Sm2（Co, Fe, Cu, Zr）17 alloys

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Preparation and characterization of TiO_2/acrylic resin composite coatings on sintered NdFeB permanent magnets by electrochemical deposition

The sintered Nd Fe B permanent magnets are widely used in various industries because of their excellent magnetic and comprehensive properties. However, they are seriously hindered to further developments and applications owing to its poor corrosion resistance. In this paper,TiO2/acrylic resin composite coatings were successfully prepared on the sintered Nd Fe B permanent magnets by electrochemical deposition for the first time, and the corrosion behaviors were investigated by using immersion testing and potentiodynamic polarization tests. It is found that the coating is a composite, being composed of polymerized acrylic resin as the matrix and nano-rutile TiO2particles(-200 nm) as the reinforcements. It is about25 lm in thickness and its surface and cross-section exhibit uniform and smooth with no pores, cracks, and other defects. Compared with those of the uncoated Nd Fe B magnets, the weight loss of the coated samples immersed in H2SO4 solution reduces by two orders of magnitude,corrosion current density decreases by four orders of magnitude, and the corrosion potential of the coated sample is shifted in the noble direction by 400 m V. The mechanisms of corrosive resistance enhancement were discussed.