烧结Nd-Fe-B磁体晶界扩散TbH2高温稳定性及其机理

采用涂敷方式,在烧结钕铁硼表面均匀涂敷TbH₂粉末,经过不同的扩散温度处理,制备出晶界扩散磁体。研究了晶界扩散TbH₂对烧结Nd-Fe-B磁体常温磁性能及高温稳定性的影响,并分析了磁体矫顽力提升的机理。常温磁性能研究表明,扩散磁体经过890 ℃+490 ℃工艺处理后性能达到最优,矫顽力从1 383 kA/m提升到1 988 kA/m。高温磁性能结果显示,扩散磁体200 ℃的矫顽力温度系数|β|比原始磁体降低0.032%/℃,磁通不可损失hirr比原始磁体降低21.47%,扩散TbH₂明显提高了烧结Nd-Fe-B磁体的热稳定性。分析得出,晶界扩散TbH₂磁体矫顽力提升的机理是Nd₂Fe₁₄B晶粒外延层形成了（Tb, Nd）₂Fe₁₄B核壳结构,提高了磁晶各向异性场;同时改善了磁体的微观组织结构,有效地隔绝了晶粒之间的磁交换耦合作用。      

晶界扩散Dy60Co35Ga5合金对烧结钕铁硼磁体 磁性能及热稳定性的影响

研究了晶界扩散Dy₆₀Co₃₅Ga₅合金对烧结钕铁硼磁体磁性能及其热稳定性的影响.随着扩散温度的升高,磁体的矫顽力（H_cj）呈现出先增加后减少的趋势,并在890 ℃扩散3 h,480 ℃回火5 h的工艺条件下,矫顽力达到较优,从1 209 kA/m提高到1 624 kA/m,磁体的剩磁只有轻微的下降,从1.38 T降低到1.32 T.高温下测试磁体的磁性能,原始磁体和890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的矫顽力都呈下降趋势,但晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的矫顽力在高温下要明显优于原始磁体.原始磁体及890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体在不同温度下保温2 h的不可逆磁通损失分别为63 %和45 %.且DSC结果显示,890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的居里温度（T_c）要明显高于原始磁体的居里温度,这表明晶界扩散磁体的热稳定性得到了很大的改善. XRD图谱显示,890 ℃晶界扩散磁体RE₂Fe₁₄B相的衍射峰较原始磁体向右偏移,说明Dy原子及Co原子少部分已进入主相晶粒.      

DyFe薄膜晶界扩散钕铁硼磁体的结构与磁学性能

采用磁控溅射在磁体易磁化面上沉积3μm厚度的Dy_xFe_1-x(x=30,50,80,100)合金薄膜层，并进行适当热处理制备晶界扩散型烧结钕铁硼磁体。当Fe含量为20%(原子分数)时，Dy₈₀Fe₂₀扩散磁体在基本不影响剩磁的情况下矫顽力能够达到15.70 kOe,接近Dy扩散磁体矫顽力，性价比更高。微观结构分析表明，重稀土元素Dy沿晶界相向磁体内部扩散的同时发生了晶格扩散，在晶粒表层生成了磁晶各向异性场更强的(Nd, Dy)₂Fe₁₄B硬磁壳层，因而磁体矫顽力增强。Dy扩散磁体经典核壳结构出现于100μm～300μm之间，且有效扩散深度小于500μm,而Dy₈₀Fe₂₀扩散磁体在100μm处便出现了明显的核壳且壳层可延续至500μm以上，说明Fe合金化可以有效缓解Dy在扩散磁体表面的聚集并提高有效扩散深度。在任意温度区间内，Dy₈₀Fe₂₀扩散磁体的α_B     

高矫顽力混合稀土永磁体的微结构与磁性能

利用高丰度混合稀土制备永磁材料不仅可以有效降低成本,同时可促进稀土资源的平衡利用。本研究采用晶界扩散工艺制备了高矫顽力混合稀土永磁体,研究了重稀土Tb对混合稀土永磁体磁性能及微结构的影响。研究发现,当晶界扩散热处理为880℃、8 h时,磁体表现出优异的磁性能,矫顽力由660.12 kA/m增长至1 248.13 kA/m,并且磁体剩磁仍然保持在1.29 T。Tb元素的扩散使混合稀土扩散磁体的主相晶粒边缘形成了(Tb,RE)₂Fe₁₄B核壳结构,这不仅增强了主相晶粒边缘的磁晶各向异性场,而且阻断了晶粒之间的磁耦合作用,抑制了反向畴形核的长大,提高了磁体的矫顽力。     

Nd-Fe-B磁体掺杂Tb-Fe-B制备高性能大块永磁体

应新能源大型设备器件需求,制备兼具高剩磁、高矫顽力的大块永磁材料成为当前研发重点。不同于晶界扩散技术(GBDP),采用双合金工艺(Nd-Fe-B磁体掺杂Tb₁₉Fe₇₅B₆)制备的多主相(Nd, Tb)-Fe-B烧结磁体,不仅可实现高剩磁与高矫顽力而且体型可控,体现出更高的实用价值。微组织分析显示,掺杂Tb₁₉Fe₇₅B₆使得磁体晶界优化并在Nd₂Fe₁₄B晶粒表层形成(Nd, Tb)₂Fe₁₄B壳层,结合Tb₂Fe₁₄B相的存在,矫顽力得以显著提升。而导致多主相(Nd, Tb)-Fe-B磁体同时实现高剩磁与高矫顽力,主要归因于微结构中Tb₂Fe₁₄B单晶与Nd₂Fe₁₄B单晶共存所触发的界面耦合效应。该研究结果为制备高性能大块永磁材料提供...     

晶界扩散Dy–Al–Ga对钕铁硼磁体的磁性能和微观组织的影响

通过晶界扩散Dy₇₀Al₁₀Ga₂₀合金研究了烧结Nd-Fe-B磁体的磁性能和热稳定性能.用NIM-500C高温永磁测量仪和MLA650扫描电镜测出了磁体在扩散前后的磁性能和微观组织的变化.结果表明，在Dy₇₀Al₁₀Ga₂₀合金扩散热处理后，磁体矫顽力从原始的1 080.968 kA/m显著提升到1 671.600 kA/m，提升幅度约为55 %，而剩磁下降很少. Dy、Al、Ga元素在晶界处扩散，很好地隔绝了磁交换作用，提升矫顽力. SEM图显示在扩散Dy₇₀Al₁₀Ga₂₀合金后，可以很明显地看到晶粒外延层有一层灰色的壳层包覆着主相晶粒，很好地起到了隔离晶粒的磁交换作用. XRD显示主相的峰普遍往右偏移，这归因于重稀土元素Dy进入晶粒外延层形成（Nd, Dy）₂Fe₁₄B核壳结构. Dy的原子半径比Nd小，导致峰往右移.      

烧结钕铁硼磁体晶界扩散Dy/DyFe工艺研究

研究了晶界扩散工艺在烧结钕铁硼中的应用,采用晶界扩散渗Dy/Dy Fe合金的方法,将重稀土元素Dy扩散到烧结钕铁硼磁体内部。在高真空6×10-3Pa下,900℃×3.5 h进行扩散,再在2×102Pa,530℃×3 h下进行回火。选择性地进行追加热处理。研究了此种工艺对烧结磁体的磁性能、磁通不可逆损失和微观组织的影响。结果表明对磁钢进行晶界扩散Dy,使矫顽力增幅为15.69%。通过晶界扩散DyFe使矫顽力增幅为22.40%。晶界扩散Dy后的磁钢在160℃/1h下,磁通不可逆损失从6.3%下降到1.1%,在180℃/2h下,磁通不可逆损失从22.6%下降到6.3%。在一定的热处理条件下,重稀土元素择优分布在主相和晶界相的交界处,这种改性的晶界结构和成分提高了各向异性场,大幅提高磁体的矫顽力和耐热性。     

镝扩渗对烧结钕铁硼磁体组织结构与磁性能的影响

对比研究了38UH、42SH和N50薄片状钕铁硼磁体晶界镝扩渗前后的组织结构与磁性能,发现经过镝扩渗处理后磁体的矫顽力提高了400 kA·m-1以上,而剩磁几乎不变,最大磁能积因为矫顽力和方形度的提高而提高。经组织结构分析认为,钕铁硼磁体晶界镝扩渗提高矫顽力主要是通过提高Nd₂Fe₁₄B晶粒外延层的各向异性和形核场实现的。根据Fick第一扩散定律,对磁体晶界镝扩渗进行了模拟计算,可近似得到定温热处理不同时间后渗镝深度及对应的镝的质量浓度及质量分数。      

(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.      

高Dy含量烧结Nd-Fe-B的晶界扩散处理研究

研究了晶界扩散处理对高Dy含量烧结Nd-Fe-B磁体性能和结构的影响。经蒸镀渗Dy晶界扩散处理,高Dy含量Nd-Fe-B磁体的矫顽力从1 713 kA/m提高至2 161 kA/m,而剩磁和最大磁能积基本没有下降,处理后磁体内Dy平均质量分数仅增加0.30%。不同深度片层分析表明,虽然磁体近表面片层比中心片层的Dy含量高,但是片层间矫顽力相差较少,而且所有片层的矫顽力均远高于未处理磁体片层的矫顽力。电子探针Dy元素面分布结果显示,在未处理高Dy含量磁体的晶界与主相中均存在Dy元素富集区且富集浓度较低,而经扩散处理后,晶界富Nd相中的Dy富集区浓度及所占比例明显提高;包括磁体芯部在内,磁体内大部分角隅处富Nd相内Dy含量明显增加,进一步提高了高Dy含量磁体内部各处的矫顽力。     

晶界扩散Tb对烧结Nd-Fe-B组织与磁性能的影响

用磁控溅射法在烧结Nd-Fe-B磁体表面沉积Tb金属薄膜并进行晶界扩散处理,对比经不同热扩散温度及时间处理后的磁体组织和磁性能变化.结果 表明,925℃×10 h+500℃×2 h为最佳晶界扩散工艺,可将磁体矫顽力提高到1630.9 kA· m-1,较原始磁体提升50％,同时剩磁和磁能积无明显下降,磁体仍具有较高的退磁...     

Characterization of Microstructure and Magnetic Properties of NdFeB Magnet with Dy, Al and Cu Additions

A new alloy of Nd33.5Dy0.99Febal.Al0.52Cu0.1B1.15 (%, mass fraction) was fabricated by powder metallurgy. The effects of Dy, Al and Cu additions on the microstructure and magnetic properties of sintered NdFeB magnet were investigated. The additions of Dy, Al and Cu are effective to refine grains and improve coercivity. Moreover, suitable amounts of Dy, Al and Cu lead to a demagnetization curve with good rectangularity. It is found that the sintered NdFeB magnet has relatively high magnetic performance of Br=12.17kGs, jHc=13.52kOe and (BH)max=34.71MGOe. The sintered NdFeB sample was examined by magnetic force microscope which revealed the domain structures at the surface. It is revealed that the mean Nd2Fe14B grain size is significantly larger than the average scale of the magnetic contrast. An explanation about this is that most Nd2Fe14B grains in sintered NdFeB alloy are dominated with the muhidomain structures when the magnet is in thermally demagnetization state.     

Effect of aluminum on microstructure and magnetic properties of sintered Nd-Fe-B magnets processed by grain boundary diffusion of Tb-Al

The grain boundary diffusion process(GBDP) of Tb can improve the coercivity of sintered Nd-Fe-B magnets.In this study,the effect of AI on the diffusion of Tb in the GBDP was investigated.The content of diffused Tb-Al was precisely controlled by adjusting the magnetron sputtering process.The Tb equivalent of Al was also studied.Results show that AI promotes the diffusion of Tb deeper into the magnet,reducing the thickness of the shell in the core-shell structure.This study is helpful for further ...     

Improvement of microstructure and coercivity for Nd-Fe-B sintered magnets by boundary introducing low melting point alloys

Different from the grain boundary diffusion process(GBDP),which is suitable for modifying thin magnet,a green-pressing agents permeation process(GAPP) that uses low melting point alloys was applied to the Nd-Fe-B green compact with a thickness over 15 mm to reconstruct the boundary microstructure of a sintered Nd-Fe-B magnet.The coercivity increases from 12.3 kOe for the sample free of Pr_(80)Al_(20) to16.8 kOe for the sample with 2 wt% Pr_(80)Al_(20).By further increasing the Pr_(80)Al_(20) content to 3 wt%,the coercivity increases slightly,but the remanence and H_k/H_(cj) deteriorate obviously.The optimal comprehensive properties of H_(cj)=16.8 kOe,B_r=13.4 kG and H_k/H_(cj)=0.975 are obtained at 2 wt% Pr_(80)Al_(20),since matrix phase grains are separated by relatively continuous thin grain boundary layers,which weaken the magnetic coupling between adjacent grains.The coercivities of the samples from the GAPP that use2 wt% Pr_(80)Al_(20),Pr_(70)Al_(30) and Pr_(60)Tb_(20)Al_(20) alloys,respectively,can be enhanced to a large extent.However,the coercivity of the magnet reconstructed with Pr_(80)Al_(20) is lower than that of the sample with Pr_(60)Tb_(20)Al_(20) but is higher than that of the sample reconstructed with Pr_(70)Cu_(30) alloy.Moreover,the coercivity of the sample from the GAPP using 2 wt% Pr_(80)Al_(20) is much higher than that of the sample from the GBDP,which is due to a nearly uniform boundary microstructure from the surface to the interior of the thick magnet from the GAPP,thus providing new insights into the fabrication of thick and bulky permanent magnets with high coercivity.     

Effects of grain boundary diffusion process on magnetic properties enhancement and microstructure evolution of hot-deformed Nd-Fe-B magnets

Grain boundary diffusion(GBD) process is an important approach for producing Nd-Fe-B magnets with high coercivity and high thermal stability.The GBD for hot-deformed Nd-Fe-B magnets with nanocrystalline micro structure is more complicated compared to sintered magnets.Here,we investigated the effects of different GBD methods,i.e.,intergranular addition(in-situ GBD 1#),in-situ GBD from magnet surface during hot pressing and hot deformation(in-situ GBD 2#),and conventional GBD,on the magnetic prope...     

Optimization of core-shell structure distribution in sintered Nd-Fe-B magnets by titanium addition

In view of the uneven distribution of the core-shell structure of sintered Nd-Fe-B magnets after grain boundary diffusion,this study proposes to use high-melting-point and reactive element titanium(Ti) as an additive to increase the diffusion channels and to enhance the diffusion of heavy rare earth elements along the grain boundary phase.By adding Ti element,the diffusion depth and hence the intrinsic coercivity of magnets are increased significantly.The addition of Ti increases the coercivity ...     

Oxide evolution in NdDy-Fe-B magnet during aging process

Sintered NdDy-Fe-B magnets were made from strip cast flakes by powder metallurgy method. For the magnet with 6wt.% Dy substituted Nd, a remarkable coercivity increase of 70% was obtained after aging at 900°C for 2h and a high coercivity of 23.5 kOe was achieved after aging at 520°C for 2h. The average diameter of the oxide particles decreased during the following 900°C aging treatment. Dy and O diffusion from oxide particles to Nd-rich phase during the aging process was observed. The oxide evolution and Dy element diffusion were helpful to the coercivity enhancement.     

Effects of grain boundary diffusion of PrCu alloy on microstructure and coercivity of hot deformed(Nd,Ce)-Fe-B magnets

The technology of using high abundance rare earth element Ce in permanent magnets has attracted many concerns.In this work,the magnetic properties and microstructures of hot deformed(Nd_(1-x)Ce_x)_(13.8)Fe_(76.1)Co_4 Ga_(0.5)B_(5.6) magnets and a selective magnet treated with PrCu grain boundary diffusion process(GBDP) were investigated systematically.It is found that Ce is beneficial to improving the plastic deformation ability of NdFeB magnets.The strongest c-axis orientation is achieved in the HD magnets with Ce concentration of x=0.3,resulting in good comprehensive magnetic properties of B_r=13.00 kGs,H_(cj)=10.12 kOe,(BH)_(max)=38.42 MGOe.Based on that,the GBDP was implemented on the magnets with the best orientation using Pr_(68)Cu_(32) ribbons and the magnetic properties of B_r=12.87 kGs,H_(cj)=15.65 kOe,(BH)_(max)=37.48 MGOe were obtained.The results of composition distribution and Curie temperature test of the GBDPed magnets illustrate that Pr diffuses into the(Nd,Ce)_2(Fe,Co)_(14)B grains to substitute Ce,which not only improves the Curie temperature of the grains,but also enhances the magnetic performance of the magnets.Through GBDP,the thermal stability of magnets has also been improved.