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     

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。      

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。     

晶界扩散中Tb对烧结NdFeB磁体微观组织和磁性能的影响

通过晶界扩散技术提升烧结钕铁硼(NdFeB)磁体矫顽力的方法已获得广泛应用,为了研究重稀土磁粉对磁体综合磁性能的影响,本文采用喷涂扩散的方法将重稀土Tb含量为6.0%(质量分数)的磁粉作为复合扩散源的一部分进行晶界扩散并制备了高性能烧结NdFeB磁体。结果表明,当主扩散源占比为60%(质量分数)时,Nd₄₀Tb₆₀对应扩散磁体的矫顽力最高达到21.52 kOe,矫顽力增幅明显。经过微观组织结构和XRD表征分析,重稀土元素Tb沿晶界相扩散进入磁体内部的同时发生了晶格取代反应,可在晶粒表层生成磁晶各向异性场更强的(Nd,Dy/Tb)₂Fe₁₄B硬磁相,显著增强了磁体矫顽力。当主扩散源占比为20%、40%和80%(质量分数)时,Nd₈₀Tb₂₀,Nd₆₀Tb₄₀和Nd₂₀Tb₈₀对应扩散磁体的矫顽力增幅较小,其中Nd₈₀Tb₂₀扩散...     

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。     

DyAl合金薄膜在NdFeB基体上真空热扩渗行为的研究

采用直流(DC)磁控溅射的方法,在烧结NdFeB磁体表面制备了DyAl合金薄膜,镀膜样品经真空热扩渗(800℃×6h)和时效处理(900℃×2.5h+490℃×5h),研究了样品的微观结构组织与磁性,并对Dy、Al元素在基体中的真空热扩渗行为进行了探讨。结果表明,随着DyAl合金薄膜厚度的增加,磁体的内禀矫顽力Hcj相应提高,内禀矫顽力Hcj提高176kA/m(2.2kOe)。通过对样品微观组织结构观察发现,Dy和Al元素沿晶界富Nd相优先扩散,大量集中分布在主相晶粒表层和富Nd相交界处,不仅改善了晶界表面浸润性,也改变了主相晶粒表层合金成分和微结构,这种晶粒表面与晶界相的改性导致烧结NdFeB磁体的内禀矫顽力Hcj提高。     

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曲线方形度。晶界扩散处理后磁体取向度有所提高,主相晶粒表面形成了明显的富Tb壳层结构,其厚度随离开磁体表面距离的增加逐渐变薄,随热扩散温度升高和时间延长逐渐增厚。长时间热扩散处理使磁体内形成沿晶界分布的连续薄层富Nd相,将主相晶粒彼此分隔,有效降低磁性相颗粒间交换耦合作用。能谱(EDS)分析表明,适当的热扩散工艺可使Tb元素扩散至磁体芯部,渗透厚度4 mm的磁体。     

Nd,Dy含量对高磁能积烧结NdFeB磁性能和耐蚀性影响

稀土Nd、Dy成分含量变化对高能积磁体磁性能和耐腐蚀性有重要影响.结果表明:当Nd含量小于12.77%(体积分数,下同)时,磁体中富Nd相过少,不能很好地去磁交换耦合作用,并导致合金烧结时收缩量少,密度过低.当Nd含量超过12.77%时,形成较多的富Nd相,能很好地隔离主相晶粒起去磁交换耦合作用,促进矫顽力提高,同时磁能积也有比较大的提高,但形成的过量晶间相增加了易腐蚀阳极含量,加剧了晶间腐蚀.添加Dy提高了主相的磁晶各向异性场,细化了主相晶粒,使磁体矫顽力增大,并且添加Dy能提高阳极过电位,有利于磁体性磁能和耐蚀性能的提高.     

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.     

晶间合金化Ga元素对烧结Nd-Fe-B磁性能与显微组织的影响

用晶间合金化方式直接在(NdPr)29.6(FeCuZr)69.2B1.0粉中加入0.3%Ga(质量分数,以下同),磁体的内禀矫顽力从943.5kA/m提高到1181.0kA/m。分别用晶间合金化方式和传统合金化方式在(Nd-PrDy)30.0(FeCuZr)69.0B1.0中加入0.2%Ga,前者的内禀矫顽力达到1224.0kA/m,远高于后者的971.5kA/m。显微组织结构分析表明:用晶间合金化方式加Ga后改善了边界结构,没加Ga时晶粒边界不平直,晶界处缺陷较多;加Ga后晶界平直光滑,Ga主要分布在晶界,而晶内Ga含量极低。     

工业生产高综合性能烧结 Nd-Fe-B永磁关键技术研究

通过优化合金成分设计和改进合金铸锭按需分配技术、磁场取向成型技术以及烧结技术，应用全部国产设备与国内通用的工业生产烧结Nd-Fe-B永磁的原材料，避免使用镓等稀有贵重金属元素，实现了N45H烧结Nd-Fe-B磁体的工业化生产，其典型磁性能为Br=1.386T(13.86kGs),BHc=1059kA/m(13.32kOe),JHc=1418kA/m(17.83kOe),Hk=1357kA/m(17.06kOe),(BH)max=364kJ/m^3(45.8MGOe)。，SEM观察和XRD分析结果表明，制造的N45H烧结Nd-Fe-B磁体具有良好的取向度和晶粒细小而均匀的显微组织。     

Enhancement of terbium efficiency by gallium and copper co-doping in (Pr,Nd)-Fe-B sintered magnets

It is well known that Tb substitution for (Pr, Nd) in (Pr, Nd)-Fe-B based sintered magnetic materials is an effective way to increase intrinsic coercivity, but it is not quite clear whether the increment depends on the different matrix phases with various doping ingredient or not, which is essential to develop high quality magnets with high coercivity more efficiently and effectively with economic consumption of expensive Tb and other costly heavy rare earths. In this paper, we investigated the efficiency of Tb substitution for magnetic property in (Pr, Nd)-Fe-B sintered permanent magnets by co-doping Ga and Cu elements. It is shown that Ga and Cu co-doping can effectively improve the efficiency of Tb substitution to increase the thermal stability and the coercivity. The intrinsic coercivity increases up to 549 and 987 kA/m respectively by 1.5 wt% and 3.0 wt% Tb substitution in Ga and Cu co-doped magnets while the intrinsic coercivity increases up to only 334 and 613 kA/m respectively by the same amounts of Tb substitution in non-Ga and low-Cu magnets. In other words, it demonstrates that there is about 329–366 kA/m linear equivalent enhancement of intrinsic coercivity by 1.0 wt% Tb substitution for (Pr, Nd) in Ga and Cu co-doped magnets. The temperature coefficients of both intrinsic coercivity β and remanence α at 20–150 °C by 3.0 wt% Tb substitution for the magnets with Ga and Cu co-doping are −0.47%/K and −0.109%/K respectively, and in contrast those values are −0.52%/K and −0.116%/K respectively for the non-Ga and low-Cu magnets. It is the principal reason for more efficient enhancement of magnetic property by Tb substitution in the Ga and Cu co-doped magnets in which Tb atoms are expelled from triple junction phases (TJPs) to penetrate into the grain boundary phases (GB phases) and thus modify the grain boundary. It is prospected that the efficiency of Tb substitution would rely on different matrix phases with various doping constituents.     

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。      

Improvement in magnetic properties,corrosion resistance and microstructure of Nd–Fe–B sintered magnets through intergranular addition of Tb68Ni32

New energy vehicles and offshore wind power industries have a high demand for sintered Nd–Fe–B magnets with high intrinsic coercivity and high corrosion resistance. In this study, the magnetic properties, anticorrosion properties, and microstructure of Nd–Fe–B sintered magnets with the intergranular addition of low-melting-point eutectic Tb₆₈Ni₃₂ alloy powders were investigated. The aim is to determine if the addition of Tb₆₈Ni₃₂ can improve these properties. A low melting-point eutectic alloy Tb₆₈Ni₃₂ powders was prepared as a grain boundary additive and blended with the master alloy powders prior to sintering. The coercivity of the resultant magnets gradually increases from 1468 to 2151 kA/m by adding increasing amounts of Tb₆₈Ni₃₂. At the same time, the remanence first increases and then slightly decreases. After studying the microstructure and elemental composition of the Tb₆₈Ni₃₂ added magnets, it is found that the significant increase in coercivity and the negligible reduction in remanence is due to densification, improved grain orientation, a uniform and continuous boundary phase distribution, as well as the generation of a (Nd,Pr,Tb)₂Fe₁₄B “core–shell” structure surrounding the main-phase grain. Moreover, the corrosion resistance of the magnet is greatly improved owing to the enhancement of electrochemical stability, as well as the optimization of the distribution and morphology of the intergranular phase.     

Coercivity enhancement of nanocrystalline hot-deformed Nd-Fe-B magnets by low-melting eutectic MM-Cu(MM=La,Ce,Pr,Nd) alloys addition

MM_(85)Cu_(15)(MM = La,Ce,Pr,Nd) eutectic alloys were added into the hot-deformed Nd-Fe-B magnets to enhance the coercivity.It is found that three endothermic peaks occur on the differential scanning calorimetry curve of the MM-Cu melt-spun ribbons at 432.2,451.1 and 516.5℃.The peaks substantially correspond to three types of MM-Cu low-melting eutectic phase.The coercivity of magnets increases when the MM-Cu content is lower than 4 wt%,and then keeps almost no change with the content further increasing to 5 wt%.The coercivity of the hot-deformed magnets with 4 wt% and without MM-Cu addition is 948 and 683 kA/m,respectively.Nearly all the platelet-shaped grains are isolated by the thickened intergranular phase after MM-Cu addition.Moreover,the average grain size of the magnets with MM-Cu addition decreases compared with that of the magnet without MM-Cu addition.Scanning electron microscopy images show that the areal fraction of the RE-rich grain boundary phase increases from 8.6% to 15.1% after MM-Cu addition.The La,Ce together with Cu and Ga aggregate at the grain boundary regions separating neighboring grains and smoothing the grain boundaries.Therefore,both the thickened grain boundary and decreased mean grain size result in the enhancement of coercivity after MM-Cu eutectic alloy addition.