贫稀土钕铁硼合金与Nd_(67)Cu_(33)混粉热变形磁体组织演变过程及其对磁体矫顽力的影响

分别真空感应快淬贫稀土钕铁硼合金Nd_(11.5)Fe_(81.8)B_(6.0)Nb_(0.7)与Nd_(67)Cu_(33)薄带,然后制备Nd_(67)Cu_(33)含量0,3%,6%,9%,12%(质量分数)的混粉热变形磁体,分析讨论了贫稀土钕铁硼合金与Nd_(67)Cu_(33)混粉变形磁体中组织演变过程及其对磁体矫顽力的影响。研究结果表明,在热变形过程中当变形量由0增到30%时,混粉热变形磁体中Nd-Cu的扩散导致与之相邻区域的α-Fe晶粒尺寸减小、局部出现富稀土相、2∶14∶1相中稀土含量部分补偿性增加,整个磁体中α-Fe相体积分数减少、2∶14∶1相与软磁相α-Fe交换耦合作用增强,混粉热变形磁体的矫顽力随变形量的增加而增大;当变形量进一步增加,在双相磁体中富稀土相消失,2∶14∶1相和α-Fe相晶粒尺寸增大,一旦α-Fe晶粒尺寸超过交换耦合的临界尺寸将导致双相交换耦合作用恶化,2∶14∶1相晶粒尺寸增大导致其对磁体矫顽力的贡献降低,整个混粉热变形磁体的矫顽力随变形量的增加而大幅度下降;当变形量达到70%时,混粉热压热变形磁体随Nd_(67)Cu_(33)添加量的增加尽管2∶14∶1等效平均晶粒尺寸增大但磁体的矫顽力不断提高,原因在于随Nd_(67)Cu_(33)的增加磁体分别出现α-Fe消失、富稀土晶界相出现、且富稀土晶界相体积分数增大,富稀土晶界相的去磁耦合作用增强。     

热变形温度对Nd14Fe80B6磁各向异性的影响

在850～880℃真空热变形4min、变形量70%制备了Nd14Fe80B6各向异性磁体,实验结果表明随着热变形温度的提高,磁体的各向异性先上升后降低,870℃热变形时磁体的(006)晶面峰为X衍射图谱的主峰、(004)相对极密度最大值达到130.01、I(006)/I(105)为1.88,获得(006)磁织构,磁体的饱和磁化强度达到1.453T。如热变形过程消除平均宽度为25μm的带状组织,减少与热变形压力垂直的片状晶之间夹角为19°左右的局部片状晶,则磁体的各向异性可望进一步提高。Nd2Fe14B相在热变形过程中从等轴晶变形为片状晶,且磁体宏观变形量≥65%时,才能形成(006)磁织构,局部富稀土相只起到有利晶粒滑移、有利片状晶形成的作用。细化热变形磁体的片状晶厚度可使磁体具有高矫顽力、高剩磁与饱和磁化强度之比值。850℃热变形Nd14Fe80B6磁体的片状晶平均厚度为76nm,磁体的矫顽力为450.6kA/m,Mr/Ms为0.92。     

晶粒尺寸对软-硬磁性晶粒间有效各向异性的影响

以软磁性相α—Re和硬磁性相Nd2Fe14B为例，研究了软—硬磁性晶粒间的交换耦合相互作用和有效各向异性随晶粒尺寸和软、硬磁性晶粒尺寸比(Ds：Dh)的关系，软—硬磁性晶粒间的有效各向异性常数可以用软、硬磁性相的平均各向异性常数的统计平均值表示，当晶粒尺寸大于其铁磁交换长度时，晶粒分为有、无交换耦合两部分，无交换耦合部分的各向异性常数为通常的K1，而耦合部分的各向异性常数随到晶粒表面的距离而变化，研究结果表明：软—硬磁性晶粒间的有效各向异性随晶粒尺寸的减小而下降，随着软、硬磁性晶粒尺寸比值(Ds：Dh)的减小而增加，为使软—硬磁性晶粒间的有效各向异性常数Keff保持较高的值，应控制硬磁性晶粒大于35nm，软磁性晶粒尺寸为10nm左右。     

Ga对HDDR磁粉热变形磁体磁性能和微观结构的影响

利用HDDR工艺制备出Nd32FebalBGax(x=0.0、0.2%、0.4%、0.6%、0.8%(质量分数))磁粉,并且对HDDR磁粉进行热压/热变形处理制备出全密度各向异性磁体。研究了热变形温度和Ga含量对Nd-Fe-B热变形磁体磁性能的影响,观测了不同Ga含量热变形磁体的微观结构,探讨了微量元素Ga的添加对用HDDR磁粉制备的热变形磁体微观结构和磁性能的影响机制。研究发现,Ga的添加能够明显减小热变形磁体的主相晶粒尺寸,改善磁体的微观织构,并可以同时提高热变形磁体的剩磁和矫顽力。当Ga含量为0.6%(质量分数)时,热变形磁体的磁能积达到最大值228.3kJ/m3。     

各向异性致密(NdDy)_(11.5)Fe_(81.5)Nb_1B_6磁体的制备

采用热压热变形技术,制得了各向异性致密(NdDy)11.5Fe81.5Nb1B6+2%(质量分数)Zn磁体,并研究了热压及热变形磁体的微观结构以及不同形变量对磁体磁性能和微观结构的影响。结果表明,Zn的添加使热压磁体磁性能下降,但使热变形磁体磁性能大幅增加;热变形磁体磁性能的增加是由于良好c轴取向和微观结构的形成。此类磁体磁性能和微观结构随形变量的增加表现出与传统磁体类似的规律,即剩磁增加、矫顽力下降,c轴取向不断增强。尽管如此,在热变形的起始阶段,由于Zn的扩散使磁体矫顽力有较大幅度增加。磁体的形变量过大达75%时,磁体磁性能会因为晶粒严重长大而下降。     

SmCo7块状纳米晶烧结磁体的制备和性能

采用放电等离子烧结技术制备了致密纳米晶SmCo6.6Nb0.4烧结磁体,研究了磁体的结构和磁性能.结果表明,烧结磁体具有TbCu7结构,说明通过SPS过程可以获得稳定的1:7相;磁体由平均晶粒尺寸约为30 nm的1:7相构成,磁体的室温矫顽力高达2.8 T,而剩磁比高达0.74,说明在纳米晶之间存在强烈的晶间交换耦合作用.烧结磁体具有良好的高温性能,773K时的矫顽力为0.48 T,矫顽力温度系数β为-0.169%/K.     

热变形温度对Nd_(14)Fe_(80)B_6磁体矫顽力的影响研究

使用X射线衍射、扫描电镜和磁滞回线仪等研究热变形温度、平均片状晶长度、单畴晶粒占比、平均片状晶厚度对热变形Nd_(14)Fe_(80)B_6磁体矫顽力的影响。结果表明,当Nd_(14)Fe_(80)B_6热变形温度超过其富稀土晶界相熔点150~170K后,磁体矫顽力从737kA/m降低到355kA/m。热变形Nd_(14)Fe_(80)B_6磁体统计平均片状晶长度L为320~500nm,单畴晶粒占比0.52~0.26,多畴晶粒的增加是热变形磁体矫顽力下降的原因。随着热变形温度的增加、变形时间的延长,平均片状晶厚度增长速度快于平均片状晶长度,对应热变形磁体矫顽力的下降。若降低变形温度在富稀土晶界相熔点附近有望提高磁体的矫顽力。     

纳米软、硬磁性晶粒间的交换耦合及其有效各向异性

以软磁性相α-Fe和硬磁性相Nd2Fe14B为例,研究了软、硬磁性晶粒间的交换耦合作用和有效各向异性常数〈Ksh〉随晶粒尺寸的变化关系。由于晶粒间的交换耦合作用,晶粒可分为晶粒内部无界面交换耦合作用影响和晶粒表面有界面交换耦合作用影响两部分,其各向异性常数为两部分的统计平均值。计算结果表明：对固定的软磁性晶粒尺寸Ds,〈Ksh〉随硬磁性晶粒尺寸Dh一致增加;对固定的Db,〈Ksj〉随Ds一致减小。为使软、硬磁性晶粒间的有效各向异性常数墨。保持较高的值,应控制硬磁性晶粒大于35nm,软磁性晶粒在10nm左右。     

各向异性热压稀土永磁体的热变形机制及微磁结构研究

重点研究制备工艺对各向异性热压稀土永磁体性能的影响,探讨了热压永磁体的热变形机理和数学描述模型,并尝试从微磁结构的角度研究各向异性纳米晶Nd-Fe-B磁体,揭示纳米晶粒之间的静磁和交换耦合相互作用、磁化和反磁化、热退磁等微观机制。获得了最佳磁性能为:Hcj=1 157 kA/m,Br=1.465 T,(BH)max=426 kJ/m3纳米晶Nd-Fe-B磁体。     

放电等离子烧结温度对热压/热变形NdFeB纳米晶永磁体磁性能的影响

采用放电等离子烧结技术制备了热压/热变形NdFeB磁体。研究了不同烧结温度对热压磁体、热变形磁体微观结构及磁性能的影响。结果表明,随烧结温度的升高,磁体密度上升,680℃时已达理论密度的99.7%;另一方面,晶粒则随温度的增加发生长大。剩磁和最大磁能积受密度和晶粒大小的交互作用,在650℃时达最大:(BH)m=129kJ/m3,Br=0.87T,Hci=914kA/m。热变形后,磁体主相晶粒的c轴逐渐转向与压力平行的方向,形成磁晶各向异性,使磁体的剩磁和最大磁能积大幅增加。热压烧结温度对热变形磁体的磁性能有着极大影响,其剩磁和最大磁能积随热压温度的升高先升高后降低,620℃热压后,热变形磁体磁性能达最大:(BH)m=339kJ/m3,Br=1.49T,Hci=576kA/m。     

Magnetic properties and microstructures of mischmetal-FeB-(Al, Ti and Al-Co) permanent magnets

The magnetic characteristics of anisotropic MM-FeB- (Al, Ti and Al-Co) permanent magnets have been investigated by using hot-pressing and die-upsetting process. The best magnetic properties obtained in these studies were H _C = 5.1 kOe, B _r = 5.4 kG with (BH)_max = 5.1 MGOe for hot-pressed MM-FeB-Al-Co magnets and H _C = 3.6 kOe, B _r = 6.7 kG, (BH)_max = 6.8 MGOe for die-upset MM-FeB-Al-Co magnets. Higher squareness of demagnetization curve was obtained in anisotropic die-upset MM-FeB- (Al, Al-Co) magnets. X-ray diffraction and STEM investigations revealed that the higher magnetic properties in die-upset magnets were resulted from alignment of the c-axis along the die-upsetting direction. The magnetic anisotropy of the die-upset magnets and the densification of the hot-pressed magnets were increased by partial substitution of Al and Al-Co for Fe.     

热模压Nd-Fe-B磁体变形过程及其模拟研究

Nd-Fe-B快淬磁粉在真空中热压,继续进行不同变形温度和不同应变率的热模压处理.通过分析不同变形温度下的热变形过程中应力一应变率关系,对热模压Nd-Fe-B磁体的热变形行为进行了研究并由此得到了描述热变形过程的关键参数.为了清楚理解晶粒边界滑移和各向异性晶粒长大在变形过程中所起的作用,利用三维有限元软件(DEFORM...     

Grain size dependence of coercivity and permeability innanocrystalline ferromagnets

Amorphous ribbons of composition Fe_74.5-xCu_xNb₃Si_13.5B₉ (x=0, 1 at.%) have been annealed between about 500°C and 900°C. This produced a series of crystallized samples with grain sizes between about 10 nm and 300 nm and with coercivities H _c and initial permeabilities μ_i varying over several orders of magnitude. The best soft magnetic properties (H _c≈0.01 A/cm and μ_i≈80×10³ ) were observed for the smallest grain sized of about 10 nm. With increasing grain size D, coercivity steeply increases following a D⁶-power law (up to D≈50 nm). H_c then runs through a maximum of H_c≈30 A/cm and decreases again for grain sizes above 150 nm according to the well-known 1/D law for polycrystalline magnets. The initial permeability was found to vary in a similar manner, essentially being inversely proportional to coercivity. The variation of the soft magnetic properties with the average grain size is discussed and compared with the predictions of the random anisotropy model and other theories for the magnetization reversal     

Exchange-coupled nanocomposites with novel microstructure and enhanced remanence by a new approach

Exchange-coupled nanocomposites with hard/soft magnetic phases are promising for the next generation of permanent magnets.Chemical methods have an advantage in controlling the nanoscale size of both phases.The nanocomposites obtained by the chemical method generally consist of a hard phase core and a soft phase shell.However,the soft-phase shell is easily oxidized leading to small enhancement of remanence.Here,a novel microstructure of Fe@FePt nanocomposites with Fe soft phase core and FePt hard phase shell has been synthesized by replacement reaction,in which the size of core and shell can be controlled below 10 nm by adjusting the ratio of Fe nanoparticles to PtCl4.Excellent exchange-coupling(single-phase-like demagnetization curves) between soft-hard phases was observed due to the precise size control of both phases,and substantial enhancements both in remanence (32 ％) and saturation magnetization (81％) were obtained in optimal nanocompistes.This work provides an alternative routine to prepare heterostructure materials with various applications.     

Examination the Grain Size Dependence of Exchange Coupling in Oxide-Based SrFe12O19/Ni0.7Zn0.3Fe2O4 Nanocomposites

Magnetic hard/soft SrFe₁₂O₁₉/Ni_0.7Zn_0.3Fe₂O₄ nanocomposites were fabricated by a two-step chemical procedure. Strontium hexaferrite NPs were synthesized via sol–gel self-propagation and then dispersed in nickel–zinc ferrite sol to prepare oxide nanocomposites by the glyoxilate precursor method. The initial product was annealed at different temperatures to study the effect of grain size on the magnetic properties of composite hard/soft ferrites. The magnetic nanoparticles (MNPs) were characterized by XRD, FTIR, TEM, and VSM techniques. Magnetic measurements indicated concave hysteresis loops for these two-phase nanocomposites due to non-complete exchange coupling at the interfaces of hard and soft ferrites. This phenomenon could be attributed to the overcritical size, 46 nm, of the hard phase, based on the critical limit of 22 nm predicted by theoretical calculation. At high annealing temperature with increasing the size of the soft phase as well as the hard phase, the dipolar interaction became dominant and the magnetic behavior of hard/soft nanocomposites approached two-phase uncoupled magnets.     

Structure and Magnetic Properties of Nd-Fe-B/a-Fe Nanocomposite Magnets by Co, Nb, Dy Substitutions

Structure and magnetic properties of the nanocomposite magnets prepared by mechanical alloying procedure with composition 55 wt pct Nd (Fe0.92B0.08)5.5+45 wt pct a-Fe, 55 wt pct Nd(Fe0.8-xCo0.12Nbx B0.08)5.5+45 wt pct a-Fe (x=0.00, 0.01, 0.03) and 55 wt pct (Nd0.9Dy0.1) (Fe0.77Co0.12Nb0.03B0.08)5.5+45 wt pct a-Fe were studied. It was found that substitution of Co for Fe could significantly improve the permanent magnetic properties of the nanocomposite magnets and typically, the maximum magnetic energy product was increased from 104.8 kJ/m3 (13.1 MGOe) to 141.6 kJ/m3 (17.7 MGOe). In contrast to the case of conventional nominally single-phase magnets, the addition of Nb results in promoting the growth of a-Fe grain and is thus unfavorable for the improvement of permanent magnetic properties of the nanocomposites. Although the addition of Dy can increase the coercivity of the magnets, the increase of magnetic anisotropy of hard phase leads to decrease of the critical grain size of soft phase. Additionally it causes the difficulty of preparing the nanocomposites because it is more difficult to control the grain size of soft phase to meet the requirement of appropriate exchange coupling between hard and soft grains.     

Novel Bimorphological Anisotropic Bulk Nanocomposite Materials with High Energy Products

Nanostructuring of magnetically hard and soft materials is fascinating for exploring next‐generation ultrastrong permanent magnets with less expensive rare‐earth elements. However, the resulting hard/soft nanocomposites often exhibit random crystallographic orientations and monomorphological equiaxed grains, leading to inferior magnetic performances compared to corresponding pure rare‐earth magnets. This study describes the first fabrication of a novel bimorphological anisotropic bulk nanocomposite using a multistep deformation approach, which consists of oriented hard‐phase SmCo rod‐shaped grains and soft‐phase Fe(Co) equiaxed grains with a high fraction (≈28 wt%) and small size (≈10 nm). The nanocomposite exhibits a record‐high energy product (28 MGOe) for this class of bulk materials with less rare‐earth elements and outperforms, for the first time, the corresponding pure rare‐earth magnet with 58% enhancement in energy product. These findings open up the door to moving from a pure permanent‐magnet system to a stronger nanocomposite system at lower costs.     

塑性加工法制备各向异性稀土永磁材料的研究进展

塑性加工是一种可制备各向异性材料并可实现近终形成形的方法,已有一系列尝试将其应用于制备高性能各向异性稀土永磁材料的研究报导.介绍了用于制备各向异性磁体或磁粉的塑性加工方法,包括热压、模压、轧制、正挤压、反挤压、等径角挤压等,和用各种塑性加工方法提高永磁材料性能的基本原理、效果,以及工业化应用进展.