Oscillatory behavior of the magnetic properties of Nd–Fe–B films with Mo and Mo–Cu additions

A series of Ta/NdFeB/Ta thin films with Mo and Mo–Cu additions embedded by alloying and by stratification have been prepared by r.f. sputtering. The influence of additions, their embedding mode, and annealing temperature on the structural and magnetic behavior of Ta/NdFeB/Ta thin films is presented. The use of additions of Mo and Mo–Cu leads to refined grain structure and improvement in the hard magnetic characteristics of Ta/NdFeB/Ta thin films. The Ta/[NdFeBMo(540 nm)/Ta films and Ta/[NdFeB(180 nm)/MoCu(dnm)] × n/Ta multilayer films present enhanced coercivities and M_r/M_s ratios in comparison with the Ta/NdFeB(540 nm)/Ta films. The stratification of Ta/NdFeB/Ta thin films with Mo–Cu interlayers leads to an oscillatory behavior of hard magnetic characteristics of the Ta/[NdFeB(180 nm)/MoCu(dnm)] × n/Ta multilayer films, when the thickness, d, of Mo–Cu interlayers varies by increments of 1 nm. When the thickness of Mo–Cu interlayers varies by increments of 2 nm the oscillatory behavior of the magnetic characteristics is not revealed. For a thickness of the Mo–Cu interlayer of 3 nm in the Ta/[NdFeB(180 nm)/MoCu(3 nm)] × 3/Ta thin films annealed at 650 °C, the c-axis of part of the hard magnetic Nd₂Fe₁₄B grains is oriented out-of-plane.     

Effect of nitrogen environment on NdFeB thin films grown by radio frequency plasma beam assisted pulsed laser deposition

NdFeB is a very attractive material for applications in electrical engineering and in electronics, for high-tech devices where high coercive field and high remanence are needed. In this paper we demonstrate that the deposition of nitrogen doped NdFeB thin films by pulsed laser deposition, in the presence of a nitrogen radiofrequency plasma beam, exhibit improved magnetic properties and surface morphology, when compared to vacuum deposited NdFeB layers. A Nd:YAG pulsed laser (3ω and 4ω) was focused on a NdFeB target, in vacuum, or in the presence of a nitrogen plasma beam. Substrate temperature (RT-850 °C), nitrogen gas pressure, and radiofrequency power (75–150 W), were particularly varied. The thin films were investigated by means of X-ray diffraction, atomic force microscopy, scanning electron microscopy, spectroscopic-ellipsometry, and vibrating sample magnetometry.     

Microstructural enhancement of high coercivity L1(0)-FePt films for next-generation magnetic recording media

The effects of substrate Ar-ion milling and Ta adhesion layer on the microstructural and magnetic properties of L1(0)-FePt films prepared on Si, SiO2, and glass substrates were investigated. It was discovered that the relatively large in-plane surface roughness of CrRu/MgO/FePt films deposited on Si substrates was due to the deformation of the CrRu layer when the composition was heated to 550 degrees C. More than an order of magnitude improvement for the in-plane surface roughness was achieved when substrate Ar-ion milling or Ta adhesion layer was incorporated into the process. While the Ta adhesion layer proved to be detrimental to the (200) growth of the CrRu layer, optimal FePt film properties with coercivity values larger than 2 Tesla and out-of-plane roughness less than 1 nm were achieved when only substrate Ar-ion milling was implemented.     

不同缓冲层和保护层对NiFe/PtMn双层膜磁性的影响

制备了以Ta和非磁性NiFeCr作为缓冲层和保护层的NiFe/PtMn双层膜,研究了它们的结构和物性,结果表明:用NiFeCr做缓冲层和保护层的NiFe/PtMn双层膜,其交换偏置场比以Ta为缓冲层和保护层的NiFe/PtMn的交换偏置场有了10%的提高;退火处理以后,以NiFeCr为缓冲层和保护层的样品的磁性层NiFe的磁矩降低要小于以Ta为缓冲层和保护层的样品的磁性层NiFe的磁矩降低.同时,XRD测量计算发现,以NiFeCr为缓冲层生长的NiFe/PtMn样品比Ta为缓冲层生长的NiFe/PtMn样品具有更好的织构,更大的平均晶粒尺寸,因而具有更好的热稳定性.NiFeCr比Ta更适合做基于Mn合金为反铁磁层的缓冲层和保护层.     

超薄Ni81Fe19薄膜的各向异性磁电阻及磁性能

利用磁控溅射方法制备了一系列超薄Ta(5nm)/Ni81Fe19(20nm)/Ta(3nm)磁性薄膜。着重研究了基片温度、缓冲层厚度对Ni81Fe19薄膜各相异性磁电阻(AMR)及磁性能的影响。利用X射线衍射仪分析了薄膜结构、晶粒取向;用四探针技术测量了薄膜的电阻率和各向异性磁电阻;用FD-SMOKE-A表面磁光克尔效应试验系统测量了薄膜的磁滞回线。结果表明:在基片温度为400℃时制备的Ni81Fe19薄膜具有较大的各向异性磁电阻效应和较低的磁化饱和场,薄膜最大各向异性磁电阻为3.5%,最低磁化饱和场为739.67A/m。基片温度为500℃制备的薄膜,饱和磁化强度Ms值最大。随着缓冲层厚度x的增加,坡莫合金薄膜的AMR值先变大后减小,在x=5nm时达到最大值。     

沉积膜厚度对NdFeB薄膜形貌和磁性能的影响

采用直流磁控溅射法,以P型单晶硅为基体材料,通过调整溅射时间制备出不同厚度的NdFeB薄膜.然后对不同厚度的薄膜运用相关仪器进行表征,结果表明,NdFeB薄膜厚度随着溅射时间的延长呈现近似线性增加,不同溅射时间段的沉积速率近似相同.矫顽力随着薄膜的厚度和Nd含量的增加而增加,薄膜中F的含量由84.01％降至81.65％,Nd含量由10.73％升至13.10％,B含量在5.25％～5.38％范围内浮动.     

NiFe/IrMn多层膜制备及MgO掺杂研究

采用磁控溅射制备了Ta/NiFe/IrMn/Ta薄膜,研究了反铁磁IrMn的溅射功率和铁磁层NiFe厚度对多层膜交换偏置场的影响。在反铁磁IrMn中插入MgO,发现MgO含量对交换偏置场有一定影响。随着MgO含量的增加,多层膜的交换偏置场逐渐增大,当MgO的含量约为2.5%交换偏置场达到最大值。随着MgO含量进一步增加交换偏置场下降。在IrMn中插入适量的MgO可以有效地增加交换偏置场。     

Effect of Heat Treatment on Microstructure and Magnetic Properties of Ce-Doped NdFeB Ribbons

The substitution for Nd by abundant element cerium (Ce) is a practical way for the comprehensive utilization of rare earth resources in NdFeB permanent magnets. In this letter, we have prepared the Ce-doped NdFeB ribbons and conventional NdFeB ribbons by melt quenching method and investigated the effects of heat treatment on the crystallization behavior, microstructure, and magnetic properties of the alloy. The results show that: (1) The crystallization behavior and the microstructural changes of the (Nd,Ce)FeB magnets are similar to the conventional NdFeB magnet when heat treatment. In addition, the Ce₂Fe₁₄B phase has a significant effect on the properties of the whole magnets. (2)The NdFeB phase and CeFeB phase are relatively close to each other after being precipitated from the amorphous phase. The coupling effect between the two phases is strong enough to weaken the effect of the addition of Ce and making the properties of the NdFeB magnets to not reduce too much after adding Ce.     

Surface modification of spherical NdFeB magnetic powders by a fluid-bed nickel electrodeposition

The spherical NdFeB magnetic powders were coated with Ni using a fluid-bed electrodeposition device. The oxidations of rich Nd phase or Fe phase were restrained after Ni coating. After annealing at 300 °C for 30 min, the magnetic properties of both coated and uncoated magnets were decreased. However, the Ni-coated powders showed better magnetic properties than the uncoated powders after the annealing. The compressive strength of bonded magnets improved after annealing due to enhancement of the adhesion between the adhesive and the surface of the magnetic powders.     

Magnetic properties and thermal stability of CoFeNi-based amorphous films

CoNiFe-based amorphous films were magnetron-sputtered to investigate their structural and magnetic properties, including annealing-induced effects and interfacial influence from additional layers of Ta and Cu. The amorphous structure was confirmed by diffraction experiments. The magnetic measurements showed a well-defined uniaxial anisotropy in plane, arising possibly from atom oblique incidence effects competing with the stray field of the magnetron. The anisotropy could be influenced by using a Ta buffer layer, though the interfacial reaction gives rise to a dead layer. A coercive force H _c of 1–2 Oe and a magnetization of 680 emu/cm³ were measured at room temperature; properties which show promise for application in magnetotunneling junction devices. Thermal analyses showed a two-stage crystallization behavior, which started at 400°C and ended at about 600°C. The Curie temperature of the amorphous phase was estimated to be about 440°C.     

用人工神经网络研究合金元素对NdFeB永磁体磁性能的影响

为了系统研究合金元素对Nd-Fe-Co-Zr-B系永磁合金磁性能的影响，采用均匀设计方法设计了Nd、Co、Zr和B的4因素6水平U18（6^4）试验方案，根据试验结果，建立了合金成分与磁性能之间的人工神经网络（ANN）预测模型。利用该预测模型获得的成分-性能的二维曲线、三维曲面及等高线图，研究了单个合金元素以及多元素间的交互作用对NdFeB磁体磁性能的影响规律。结果表明：预测结果与实测结果吻合良好，预测精度高；Nd、Zr为提高矫顽力Hcj而降低剩磁Br的元素；Co、B则对提高Br有利而对提高Hcj不利；合金元素对Hcj与Br的影响呈相反的趋势；元素间交互作用对磁性能影响显著。     

磁场热处理对NdFeB非晶快淬粉末的晶化与磁性的影响

研究了外中磁场对非晶Ｎｄ５．５Ｆｅ６６Ｂ１８．５Ｃｒ５Ｃｏ５，Ｎｄ４．５Ｆ３７７Ｂ１８．５和Ｎｄ１０．５Ｆｅｎ７０Ｂ７．０Ｚｒ２．５Ｃｏ１０粉末的晶化与磁性的影响，发现在热处理过程中加磁场可促进淬非晶粉末的晶化，使相转变在较低的温度下进行，讨论了各向异性复合纳米永磁材料可能的制备方法。     

New kind of NdFeB magnet prepared by spark plasma sintering

We have produced an anisotropic Nd/sub 15.5/Dy/sub 1.0/Fe/sub 72.7/Co/sub 3.0/B/sub 6.8/Al/sub 1.0/ magnet by the spark plasma sintering (SPS) technique and compared it with a magnet of the same composition processed by the conventional sintering method. We investigated magnetic properties, microstructure, and constituents by a B-H loop-line instrument, a scanning electron microscope, and an energy-dispersive X-ray detector, and studied the effects of processing conditions on the magnetic properties, dimensional precision, and density. We also examined the magnet's electrochemical properties in electrolytes and its corrosion behavior in oxidizing environments. We found that the microstructure of the SPS NdFeB magnet is different from that of the conventional one. In the SPS-processed magnet, the grain size is fine and uniform while the distribution of the Nd-rich phase is heterogeneous. The SPS NdFeB magnet has a maximum energy product of 240 kJ/m/sup 3/ and a coercive force of 1260 kA/m. The density of the magnet reaches 7.58 g/cm/sup 3/, and its dimensional precision is about 20 /spl mu/m. The electrochemical properties and the corrosion resistance of the SPS NdFeB magnet are better than those of the conventional one. The SPS process is a promising method for the production of NdFeB magnets with ideal overall performance.     

Properties improvement and structural optimization of sintered NdFeB magnets by non-rare earth compound grain boundary diffusion

Grain boundary diffusion using rare earth (RE)-containing compounds has recently become an effective approach for improving the coercivity and reducing the heavy RE content in sintered NdFeB magnets. Here we report the enhancement of magnetic properties and corrosion resistance of NdFeB magnets by a non-RE compound diffusion process. The Dy-free sintered NdFeB magnets were coated with an MgO layer by magnetron sputtering, followed by solid diffusion heat treatment. With the successful diffusion of MgO into the magnet, the coercivity increasing from 1094 to 1170 kA/m and the maximum energy product increasing from 240 to 261 kJ/m³, together with the enhanced temperature stability and corrosion resistance, have been demonstrated. The underlying mechanisms for these enhancements have been analyzed. Microstructural investigations show that MgO entered mainly into the intergranular regions and modified the composition and structure of the grain boundary phase. The intergranular Nd–O–Fe–Mg phases observed in the MgO diffused magnet contribute to the improved performance. The current non-RE compound grain boundary diffusion process has significance in further minimizing the use of rare earth (RE).     

表面宏微处理对塑料粘结NdFeB永磁性能的影响

本文研究了偶联剂处理ＮｄＦｅＢ磁粉及环氧树脂涂层对塑料粘结ＮｄＦｅＢ永磁体性能的影响，结果表明：（１）ＫＨ５５０包覆处理ＮｄＦｅＢ磁粉可改善Ｎｄ－ＦｅＢ磁粉的抗氧化性，提高塑料粘结ＮｄＦｅＢ的磁性能和压缩强度；（２）用偶联剂微观保护ＮｄＦｅＢ磁粉和环氧树脂涂层宏观保护相结合的办法可显著地提高塑料粘结ＮｄＦｅＢ永磁体的耐蚀性和抗高温氧化性     

高性能的尼龙1010 粘结NdFeB 永磁材料的制备

研究热塑性树脂尼龙1010 作粘结剂制备高密度粘结N dFeB 永磁材料的工艺及其对粘结 永磁性能的影响。结果表明: 快淬N dFeB 磁粉的表面状态、混炼工艺及热压成型温度、压力及时间 明显影响着尼龙1010 粘结N dFeB 永磁的性能。只有经抗氧化处理的快淬N dFeB 永磁粉, 在双辊 混炼机上, 当尼龙1010 处于半熔融状态时, 在适当短的时间混合均匀后, 才可热压制成高密度的 粘结N dFeB 永磁材料。      

The effect of Ta on structure and magnetic properties in Fe–N films

Microstructure and magnetic properties of Fe–Ta–N alloy films near the eutatic composition were studied. The four systematic alloy films with different Ta content were prepared by reactive sputtering. The dependence of structures and magnetic properties on Ta and annealing were investigated by VSM and X-ray diffraction. It is found that Ta atoms replace Fe in α-Fe lattice and have strong affinity for nitrogen, which inhibits the formation of γ-Fe₄N phase in Fe–Ta–N films. The TaN phase precipitates in grain boundaries and suppresses the growth of α-Fe(N) crystalline during annealing. Coercivity varies with the change of microstructure.     

钕铁硼器件表面电沉积铜层及性能

针对钕铁硼器件现有Ni/Cu/Ni镀层防护体系存在的磁性能衰减问题,用碱性HEDP络合剂镀液在钕铁硼磁体表面直接电沉积铜层,并在其上电镀镍,构成Cu/Ni镀层防护体系代替通常的Ni/Cu/Ni镀层体系。通过电化学测试研究镀铜液中HEDP络合剂浓度对铜沉积过程的影响;应用SEM,XRD,TEM对铜层微观形貌进行了表征;分别用热震实验和热减磁实验对铜层结合力和钕铁硼器件的热减磁性能进行测试。结果表明:镀铜溶液中HEDP对铜离子沉积过电位影响较大,铜晶粒在钕铁硼晶界处优先沉积,并以(111)晶面取向为主;钕铁硼磁体上镀铜层结构致密,与钕铁硼的结合力良好,满足SJ 1282—1977的要求;Cu/Ni镀层体系的钕铁硼热减磁衰减率相比于Ni/Cu/Ni镀层显著减小。     

NdFeB/酚醛树脂原位复合材料研究

采用原位聚合法制备了NdFeB/酚醛树脂(PF)母料,并进一步制备了粘结磁体.采用红外分析了NdFeB/PF母料的结构,并用多种方法对粘结磁体的磁性能和力学性能进行了研究.研究表明:在原位制备过程中,PF的聚合倾向于在NdFeB的表面进行,形成PF包覆的NdFeB,NdFeB磁粉进入了PF的生成体系,形成了海岛结构.比较三种工艺制备的磁体综合性能可知,采用NdFeB/PF母料粉料作粘结剂制备的磁体的综合性能最好.     

Ta additive effect on RF magnetron sputtered CoCr films

Magnetic properties for sputtered CoCrTa films (18 at.% Cr and 2.0-3.0 at.% Ta), which were deposited under various background pressures P_i, and argon sputtering pressures, P _Ar, have been examined. The perpendicular anisotropy field H_k for CoCrTa films maintains high values of 5-6 kOe in a wide range of P_i and P_Ar , as compared with that for CoCr films. In order to optimize Ta composition, magnetic properties and crystalline microstructures for Ta additive content (0-4.0 at.%) have been investigated. H_k and perpendicular coercivity H_c⊥ increase with increasing Ta concentration above 2.0 at.% Ta. C-axis orientation is improved by adding Ta to CoCr films. However, above 3.0 at.% Ta, H_c⊥ steeply decreases and domain wall motion is observed, owing to the increase in crystalline grain size. The appropriate Ta composition is 2.0-3.0 at.%