Nd-Fe-B磁体烧结过程晶粒长大行为的研究

定量描述了Nd-Fe-B磁体烧结过程晶粒长大行为，分析了烧结温度、烧结时间、合金粉末粒度及其分布对烧结过程晶粒长大的影响，讨论了烧结过程晶粒长大机制。在Nd-Fe-B磁体烧结过程开始之后的0—1h时间区段，晶粒长大迅速；随着烧结时间的延长，晶粒长大速度减小。合金粉末平均粒度增大，或者合金粉末粒度分布范围增宽，显著促进Nd-Fe-B磁体烧结过程中晶粒的长大。在Nd-Fe-B磁体的烧结过程中，存在两类晶粒长大机制，即Nd2Fe14B颗粒的溶解与析出、Nd2Fe14B颗粒的并合与长大。Nd2Fe14B颗粒的并合与长大不仅使磁体的平均晶粒尺寸增大，也使晶粒尺寸分布范围增宽，是烧结Nd-Fe-B磁体显微组织中出现异常大晶粒的根本原因。     

HDDR过程中三元和多元Nd-Fe-B合金磁畴结构的MFM研究

用磁力显微镜研究了三元Nd-Fe-B合金在HDDR过程的不同阶段(铸态、不充分吸氢歧化、充分吸氢歧化和脱氢再复合)的破畴结构。在铸态样品表面清楚地观察到了易磁化轴互相垂直的柱状晶表面的两类磁畴图型。当样品不充分吸氢歧化和充分吸氢歧化时，破畴结构明显发生变化，反映了Nd-Fe-B的分解产物NdH2，α-Fe和Fe2B及其微晶结构的变化。脱氢再复合后形成的微晶的磁畴结构则表明样品保留了铸态样品柱状晶的构型。此外，还对比研究了多元Nd-Fe-B合金在HDDR过程中的磁畴结构，并根据微磁结构分析，指出过量的Ga元素添加可抑制Nd2(Fe，M)14B相的吸氢歧化，从而导致相应HDDR粘结磁体性能降低。     

惰气熔融-热导法测定钕铁硼永磁材料中的氢

建立惰气熔融-热导法测定钕铁硼永磁材料中氢的分析方法。当氧-氢比例大于50:1时,CO对氢的测定结果产生一定的干扰,加入舒茨试剂可消除此干扰。采用标准坩埚,称样0.05g,熔融功率为2.85 kW,选择高纯镍篮和锡片做助熔剂,钕铁硼中氢释放完全。以普通钢铁参考物质建立氢校准曲线,线性相关系数r～2=0.9999,检出限为0.75μg/g。该法用于钕铁硼样品中氢的测定,测定结果与脉冲熔融飞行时间质谱-气体元素分析仪测定结果基本一致,测定结果的相对标准偏差为1.4%(n=5)。该方法可以准确测定钕铁硼永磁材料中的氢,能满足日常分析的要求。     

Nd-Fe-B/FeCo多层纳米复合膜的结构和磁性

制备了Nd₂₈Fe₆₆B₆/Fe₅₀Co₅₀多层纳米复合磁性薄膜，对溅射态和650℃退火处理15 min试样的相成分分析和微结构的观察显示，溅射态薄膜呈非晶态，经650℃退火处理15 min后，薄膜主要相成分为硬磁性Nd₂Fe₁₄B相和软磁性相FeCo(110)相.Nd₂Fe₁₄B相呈柱状，其易磁化c轴垂直于膜面，尺寸约10 nm.在硬磁性相和软磁性相之间存在少量富Nd相和非晶态，富Nd相大小约7 nm.磁性测量和分析表明，1)该系列薄膜退火态具有垂直于膜面的磁晶各向异性.2)对于固定厚度(10 nm)层Nd-Fe-B和不同厚度(t_FeCo=1—100 nm)层FeCo多层纳米复合膜,剩磁随软磁相FeCo 厚度的增加快速增加，而矫顽力则减小.当t_FeCo=5 nm时，最大磁能积达到200 kJ/m³. 3)硬磁相Nd-Fe-B层和软磁相FeCo层之间交换耦合导致剩磁和磁能积增强. 关键词： Nd-Fe-B/FeCo多层纳米复合膜 交换耦合 磁各向异性     

Hot deformation in nanocrystalline Ndben Feben B backward extruded rings

Radially oriented Nd-Fe-B rings are prepared by backward extrusion of fine grained melt-spun powder. Melt-spun powder with the nominal composition of Nd_30.5Fe_bal.Co_6.0Ga_0.6Al_0.2B_0.9 (wt%) is used as starting material. The effects of process variables, such as deformation temperature (T_d), strain rate (ε) and height reduction (Δh%), on the magnetic properties of the rings are investigated. A scanning electron microscope (SEM) equipped with an energy spectrum device is used to study the metallograph and microfracture of the extruded rings. The B_r and (BH)_max reach the optimum values at T_d=800℃, ε =0.01 mm/s, and Δh% =70%. It is found by SEM observations that the particle boundaries, which seemingly correspond to the interfaces of the starting melt-spun powders, emerge after the corrosion of metallography specimens. This is helpful for studying the effects of powder-powder interface on the local deformation and deformation homogeneity in the rings. For different spatial positions of the extruded rings, there are characteristic metallographies and microfractures. The upper end of the rings has the least deformation and worst texture, and therefore the worst magnetic properties. The magnetic properties in the radial direction increase slightly along the axis from the bottom to the middle, then steeply decrease at the upper end of the ring. The deformation and the formation-of-texturing processes are discussed. The deformation and the texturing formation of melt-spun Nd-Fe-B alloys probably involve grain boundary sliding and grain rotation, the solution-precipitation process and preferential growth of Nd₂Fe₁₄B nanograins along the easy growth a-axis.     

High coercive Nd-Fe-B magnets fabricated via two-step sintering

The fabrication of Nd₁₁Dy₄Fe_76.5TM_2.5B₆ (TM=Co, Cu, Al, and Nb: at%) sintered magnets via a two-step sintering process was demonstrated. A densification of greater than 99% was achieved using the two-step sintering of the Nd-Fe-B powder. This process produced a sample with an average grain size of 6.2 μm in the Nd₂Fe₁₄B phase, resulting in an enhancement of the coercivity compared to that of the isothermally sintered sample. The suppression of grain growth was considered to be affected by the relatively low temperature during the two-step sintering and by the presence of a B-rich phase at the triple junction. Consequently, the two-step sintering process led to suppression of grain growth and a uniform grain size distribution, which resulted in improved magnetic properties, in particular in the intrinsic coercivity.     

新型钕铁硼电磁阻尼演示仪

利用稀土永磁材料钕铁硼（Ｎｄ－Ｆｅ－Ｂ）设计制作出一种新型电关演示仪,可演示阻尼振动的三种状态（欠阻尼状态、临界阻尼状态、过阻尼状态）,配合投影仪使用,演示效果显著。     

2,6-二溴-4-甲基偶氮磺分光光度法测定钕铁硼合金中的钕

研究2,6-二溴-4-甲基偶氮磺(DBM-SA)与钕(Ⅲ)的显色反应,建立了测定钕铁硼合金中钕的分光光度分析方法。在2mol/L磷酸介质中,钕(Ⅲ)与DBM-SA发生灵敏的显色反应,生成配合比为1:2的蓝色配合物,其最大吸收波长为634nm,表观摩尔吸光系数为1.0×10~5L/(mol·cm)。钕(Ⅲ)的浓度在0～1.0μg/mL内符合比耳定律。该方法用于实际样品分析,加标回收率为97.6％～99.8％,测定结果的相对标准偏差为0.65％～0.82％。     

ICP-AES法测定钕铁硼永磁材料中常量元素

研究了等离子发射光谱法 (ICP AES)直接测定钕铁硼永磁材料中常量元素Nd ,Fe,B的方法。选择了合适的分析线 ,采用基体匹配法消除样品中基体元素的干扰。详细讨论了ICP AES法测定硼的“记忆效应”及其消除方法。以多点 (3个点 )标准曲线法减小测定的误差。本方法已应用于钕铁硼产品的快速检验 ,样品中Nd ,Fe,B含量测定的相对标准偏差分别为 0 6 2 % ,0 5 6 % ,0 90 %     

利用Pr_(70)Cu_(30)晶界扩散改善烧结钕铁硼废料矫顽力的研究

钕铁硼磁体制备过程中出现的部分块体废料由于矫顽力较低,性能难以满足使用要求.本文主要通过晶界扩散技术来提高废料磁体的矫顽力.采用Pr_(70)Cu_(30)合金作为扩散介质,对烧结钕铁硼废料磁体进行了晶界扩散处理,研究了扩散温度、扩散时间和回火时间对扩散后的磁体性能的影响.结果显示,800℃下扩散3 h,磁体的矫顽力从原来的7.88 kOe(1 Oe=79.5775 A/m)提升至11.55 kOe,提升幅度为46.6%,同时剩磁没有明显降低.扩散后回火对矫顽力的提升有一定的作用.800℃下扩散4h后的磁体在500℃回火3h后,最高矫顽力可达11.97 kOe,比原磁体废料提高了51.9%,接近成品磁体的水平.显微组织分析证实了晶界扩散的作用.扩散处理后的磁体中,主相晶粒间形成了连续晶间相,起到有效的磁隔离作用,有利于矫顽力的提高.研究还发现,Pr_(70)Cu_(30)晶界扩散虽然可以使磁体腐蚀电位上升,但也会增加腐蚀电流密度,不利于磁体抗腐蚀性的改善.本文工作对于提高材料的成品率具有重要意义.