Effects of Nd on the microstructure and magnetic properties of Ni-Zn ferrites

Ni_0.4Zn_0.6Fe_2−xNd_xO₄(x = 0-0.07) ferrites doped with different amounts of Nd₂O₃ were prepared using standard ceramic technique. The samples were uniaxially pressed and sintered at 1250°C for 4 h in air. The phase structure and microstructure of the samples were investigated using X-ray diffraction and scanning electron microscope, respectively. The complex permeability was measured using the impedance analyzer in the range of 1-100 MHz. The results indicate that with increasing Nd³⁺ content, the relative density and lattice parameter a of the sintered samples increase, whereas the real part of permeability (μ′) and the magnetic loss tangent (tan δ) decrease. The substitution of Nd³⁺ for Fe³⁺ forms a secondary phase on the grain boundary of the matrix, which strongly restrains the grain growth of the matrix.     

烧结(Nd,Tb)-Fe-B磁体的元素扩散、反磁化和矫顽力

采用双合金法将两种粉末混合制备烧结永磁体可提高磁体磁性能;但在烧结过程中两种粉末之间存在元素扩散,元素扩散对磁性能的影响程度需要进一步研究。本文将Nd13Fe81B6和TbHx粉末混合制备烧结磁体,Nd13Fe81B6磁体矫顽力为4.5 kOe。当TbHx混合量为3 wt.%,烧结磁体的矫顽力增加至20.0 kOe。通过热激活研究认为,磁畴壁的形核是反磁化需要经过的过程。由于热力学的原因Tb元素更容易扩散进入Nd2Fe14B主相而不是富集在晶间富稀土相。Tb元素进入主相替代Nd可形成具有更高各向异性场的(Nd,Tb)-Fe-B表层,在反磁化过程中晶粒表层磁畴壁的形核场会增加,因此矫顽力增加程度显著。但是,TbHx混合量超过5 wt.%,矫顽力增加幅度降低。对于TbHx混合量7 wt.%的磁体,元素分布显示在主相晶粒内部贫Tb区域明显增少,证实在烧结过程中更多Tb原子从晶粒表层扩散入晶粒内部,这样晶粒表层反磁化形核场的提高程度会减弱,因而磁体矫顽力增加幅度降低。本研究说明要提高双合金Nd-Fe-B磁体磁性能需进一步控制元素扩散并优化磁体的元素分布。     

富钕相对烧结NdFeB磁体耐腐蚀性的影响

研究了Nd2Fe14B单晶、传统烧结NdFeB磁体和放电等离子烧结（简称SPS）NdFeB磁体在电解液溶液中的电化学特性。采用扫描电子显微镜和电子能谱分析了磁体的微观组织成分。结果表明在3．5％NaCI溶液的极化曲线中，Nd2Fe14B单晶具有最高的电化学腐蚀电位，放电等离子烧结NdFeB磁体的腐蚀电位高于传统烧结NdFeB磁体。与传统烧结NdFeB磁体相比，放电等离子烧结NdFeB磁体富Nd相具有独特的分布形态，主相Nd2Fe14B晶粒细小、均匀，富钕相在主相晶粒边界上分布较少，主要集中在三角晶界处。这种组织结构有效地抑制了磁体沿富钕相发生晶间腐蚀的过程，磁体因此具有良好的耐腐蚀性能。此外，从不同稀土含量的烧结NdFeB磁体的高压加速实验中可以看出磁体的腐蚀速度随稀土含量的增加而增大。以上结果表明富Nd相的化学特性及其分布状态和含量是决定合金耐蚀性能的关键，它在合金中以网络状分布在主相晶粒边界上，并决定了烧结NdFeB易于发生选择性晶间腐蚀，从而导致耐蚀性差。     

Effect of Annealing on the Magnetism of the Sintered NdFeB Magnet

This paper deals with the effect of annealing on the magnetism of the sintered NdFeB magnet with a composition of Nd30B5.1Dy1.2Al0.6Nb0.7Fe62.4. Microstructural investigations of the grain size and grain boundaries with SEM were carried out. Microstructural investigations showed the presence of some Nd-rich phase in grain boundaries and main phase.The results of magnetic properties analysis shows that this non-magnetic Nd-rich phase, produced in annealing process,can increase or decrease the magnetism of the sintered NdFeB-type permanent magnet. Appropriate amount of Nd-rich phase will strengthen the pinning field and elevated the coercive force of magnet, but too many these non-magnetism phases in Nd2Fe14B main phase will decrease it. When the sintered NdFeB magnet was annealed at 3Pa and 492℃ for an hour the coercive force would raise from 915.6kA/m to l164.SkA/m, and the (BH)max from 277.7kJ/m to 349.5kJ/m. However, annealing at a non-optimized temperature at 542℃, microstructure changes in some main phase will leading the decrease of properties.     

三相烧结工艺对NdFeB磁体结构与性能的影响

本文采用Nd2Fe14B、Nd55FeBCo和Nd86FeCu53相粉末共烧结的方法制得NdFeB磁体。研究发现通过3相烧结工艺制得NdFeB磁体的晶界相比常规工艺制得NdFeB磁体的晶界相更均匀。由于晶界存在大量的Nd-Cu4、NdCo3和NdCo2相,晶界相的平均电位大大升高,超过了主相Nd2Fe14B的电位。因而NdFeB磁体发生电化学腐蚀时,电流密度大大降低,耐腐蚀性能得到了显著的改善。磁体腐蚀失重从一般工艺的60.47 mg.cm-2下降至1.2 mg.cm-2,而磁体的磁性能基本保持不变。     

Preparation and characterization of TiO_2/acrylic resin composite coatings on sintered NdFeB permanent magnets by electrochemical deposition

The sintered Nd Fe B permanent magnets are widely used in various industries because of their excellent magnetic and comprehensive properties. However, they are seriously hindered to further developments and applications owing to its poor corrosion resistance. In this paper,TiO2/acrylic resin composite coatings were successfully prepared on the sintered Nd Fe B permanent magnets by electrochemical deposition for the first time, and the corrosion behaviors were investigated by using immersion testing and potentiodynamic polarization tests. It is found that the coating is a composite, being composed of polymerized acrylic resin as the matrix and nano-rutile TiO2particles(-200 nm) as the reinforcements. It is about25 lm in thickness and its surface and cross-section exhibit uniform and smooth with no pores, cracks, and other defects. Compared with those of the uncoated Nd Fe B magnets, the weight loss of the coated samples immersed in H2SO4 solution reduces by two orders of magnitude,corrosion current density decreases by four orders of magnitude, and the corrosion potential of the coated sample is shifted in the noble direction by 400 m V. The mechanisms of corrosive resistance enhancement were discussed.     

添加Dy2O3对烧结NdFeB磁体微观结构的影响

研究了NdFeB粉末中添加1wt％Dy2O3粉末对烧结NdFeB磁体微观结构的影响，研究发现，在烧结过程中，Dy2O3中的Dy与Nd2Fe14B中的Nd发生了置换反应，Dy进入Nd2Fe14B相，形成了（Nd，Dy）2Fe14B相，提高了磁体的矫顽力。     

Effects of Ti and(or) Cu on microstructures and magnetic properties of sintered Nd-Fe-B magnets

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烧结NdFeB磁体热压变形后富Nd相的显微组织

采用热压变形法对NdFeB磁体晶间富Nd相的显微组织进行了研究,实验结果表明,NdFeB磁体经真空热压变形后,富Nd相不再平均地分布在磁体晶间,而是聚集成团块状或从磁体边缘渗出,显微组织分析表明,富Nd相主要是由α-Dd和Nd2Fe17两相组成,与Nd-Fe合金的共晶组织成分接近,对于晶间添加Al元素的磁体,Al溶入晶间形成Nd2Fe15Al2相弥散地分布在晶界上,这有益于磁体矫顽力的提高;对于晶间添加Cu元素的磁体,晶间没有发现有新相产生。     

快淬Fe3B／Nd2Fe14B永磁材料晶化行为及磁性能的研究

利用熔体快淬和晶化处理的方法制备了快淬Fe3B／Nd2Fe14B永磁材料。采用XRD，DTA，VSM等方法对合金的晶化行为和磁性能进行研究。结果表明：对于Fe3B／Nd2Fe14B熔体快淬永磁粉末，升温速率对各相的析出和分解温度有一定的影响。完全过淬的Nd4.5Fe77B18.5和Nd4Fe77Cr0.5B18.5合金熔体快淬粉在进行973K，7min晶化处理过程中，首先形成Nd2Fe23B3相，然后Nd2Fe23B3相发生分解，其产物为Fe3B／Nd2Fe14B，此后再没有发生其它的相转变。当晶化温度大于953K，保温10min后，样品的剩磁、矫顽力和最大磁能积明显提高。微量元素Cr的添加对相转变温度有影响，同时可以细化晶粒，提高矫顽力，从而改善材料的永磁性能。     

Microstructural control of and mechanical properties of mechanically alloyed tungsten heavy alloys

93W-5.6Ni-l.4Fe tungsten heavy alloys with controlled microstructures were fabricated by mechanically alloying of elemental powders of tungsten, nickel and iron by two different process routes. One was the full mechanical alloying of blended powders with a composition of 93W-5.6Ni-l.4Fe, and the other was the partial mechanical alloying of blended powders with a composition of 30W-56Ni-14Fe followed by blending with tungsten powders to form a final composition of 93W-5.6Ni-l.4Fe. The raw powders were consolidated by die compaction followed by solid state sintering at 1300°C for 1 hour in a hydrogen atmosphere. The solid state sintered tungsten heavy alloys were subsequently liquid phase sintered at 1445∼1485°C for 4-90 min. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed tungsten particles of about 6-15 μm much finer than those of 40 um in a conventional liquid phase sintered tungsten heavy alloy. An inhomogeneous distribution of the solid solution matrix phase was obtained in the two-step sintered tungsten heavy alloy using partially mechanically alloyed powders. The two-step sintered tungsten heavy alloy using mechanically alloyed 93W-5.6Ni-l.4Fe powders showed larger elongation of 16% than that of 1% in the solid state sintered tungsten heavy alloy due to the increase in matrix volume fraction and decrease in W/W contiguity. Dynamic torsional tests of the two-step sintered tungsten heavy alloys showed reduced shear strain at maximum shear stress than did the sintered tungsten heavy alloys using the conventional liquid phase sintering.     

Microstructure of explosively compacted Nd-Fe-B magnet by TEM

The microstructure of an explosively compacted Nd-Fe-B permanent magnet(Nd-Fe-B) was investigated by means of TEM and XRD. It is shown that there are three kinds of phases: Nd2 Fe14 B matrix phase, O-rich phases and Nd-rich phase with different structures and compositions in the magnet. The hard magnetic phase Nd2Fe14 B is tetragonal, which lattice parameters are determined to be a=0.88 nm and c=1.22 nm. The O-rich phase locates at the grain boundaries and the triple junctions has fcc structure whose lattice parameter is a=0. 559 nm. A dislocation is observed in this phase. It is also found that a large number of the block-shaped Nd-rich phases with hcp structure are embedded in the Nd2 Fe14 B matrix or at grain boundary. Their lattice parameters are determined to be a= 0. 395 nm and c=0. 628 nm.     

机械力驱动下Nd16Fe76B8合金氢化-歧化反应机理研究

对机械力驱动下Nd16Fe76B8合金的氢化-歧化反应机理进行了研究。通过测量球磨过程中合金的吸氢量变化,揭示了其氢化-歧化反应动力学特征。采用X射线衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)等方法,研究了球磨过程中合金的组织演变。结果表明:在球磨的最初阶段,合金只发生氢化反应,生成NdH2.7与Nd2Fe14BHy相,此后随着球磨时间的延长,氢化态合金粉末在机械球磨的作用下被激活至高能状态,并逐渐发生歧化,最终得到晶粒尺寸约10nm的NdH2.7、Fe2B、α-Fe的纳米歧化组织。     

添加Nb对Nd—Fe—B磁体温度稳定性的影响

对Nd15.15Fe78.11-xNbxB6.74(x=0,0.21,0.42,0.72,1.08,1.44)永磁体的温度特性和显微组织及两者之间的关系进行了研究，结果表明：Nb可以显著降低磁体的磙这不可逆损失，但对磁体磁通可逆部分几乎没有影响，Nb对Nd-Fe-B磁体中的作用是使晶粒均匀化，规则化，导致晶粒表面层厚度r0大幅度变薄，晶粒表面的最小形核场H11和Bloch壁的挣脱钉扎场HN增大，因而使磁体的不可逆损失降低，温度稳定性和使用温度提高。     

添加元素Dy对Nd—Fe—B永磁合金性能的影响

由于氢化制粉制备的ＮｄＦｅＢ粉末制品烧结时磁体中的晶粒异常长大,使合金的矫顽力降低。通过在ＮｄＦｅＢ合金中加入少量Ｄｙ２Ｏ３,能有效地抑制合金高温烧结时的晶粒长大,增加了各向异性很高的（Ｎｄ,Ｄｙ）２Ｆｅ１４Ｂ相,从而使合金的矫顽力得到提高,当Ｄｙ的加入量超过（摩尔分数）４％时,Ｄｙ在富Ｎｄ相晶界中分布比在基体相Ｎｄ２Ｆｅ１４Ｂ中高。     

机械合金化和添加微量Y2O3对制备细晶钨合金

采用机械合金化、添加微量Y2O3和冷等静压、液相烧结工艺制备Ф25mm的晶粒度为3～4μm的细晶93W-4.9Ni-2.1Fe(质量分数%,下同)合金棒材,研究粉末机械合金化、添加微量Y2O3、烧结温度和保温时间对合金棒材烧结致密化和显微组织的影响。结果表明:在1480℃液相烧结时钨晶粒发生明显球化,在此温度下降低保温时间对控制钨晶粒长大有较大影响,保温时间为30min时,钨晶粒尺寸为5～8μm;保温时间为60min时,钨晶粒为8～10μm。添加微量稀土氧化物Y2O3可以进一步有效地抑制晶粒的长大,降低合金的钨晶粒尺寸和提高组织均匀性,在1480℃烧结60min时,钨晶粒为3～4μm,而且晶粒尺寸分布更均匀。     

Influence of Fe and Ti addition on properties of Na<Superscript>+</Superscript>-β/β″-alumina solid electrolytes

Transition metal (Fe, Ti)-doped Na⁺–β/β″-alumina samples were synthesized via a solid-state reaction, and the sintered specimens were characterized using X-ray diffraction, scanning electron microscopy, densitometry, and impedance analysis. The results indicated that both the sintered density and β"-alumina fraction were effectively improved by doping with Fe and Ti because of the increased concentration of Al³⁺ ion vacancies in the Na⁺–β/β″-alumina. These vacancies promoted stabilization of the β″-alumina phase and densification by providing a diffusion path for Al³⁺ ions. The presence of Fe and Ti in the alumina increased the grain boundary diffusivity, thereby improving the mass transport. Thus, anisotropic grain growth occurred with increasing dopant content. However, excessive liquid-phase formation during sintering occurred when the amount of Ti was greater than 2.0 mol%, and the lowered sintered density decreased the ionic conductivity of the Na⁺-β/β″-alumina because the ionic conductivity behavior has a closer relationship to the trend of sintered density. The highest ionic conductivities of the Fe- and Ti-doped sintered specimens were 1.4 × 10^-1 S/cm (10.0 mol% Fe-doped) and 1.6 × 10^-1 S/cm (1.5 mol% Ti-doped) at 350 °C.     

烧结NdFeB磁体相的继承性研究

设计成分为Nd32.5B1.04Febal(质量分数,%),经过熔炼,制粉,成型,烧结后制备了烧结NdFeB磁体,对样品的铸锭,烧结态样品以及高温回火态样品,低温回火态样品的微观组织采用SEM进行了仔细地分析。结果显示,烧结NdFeB磁体的相具有"继承性",在熔炼中产生的α-Fe相会被烧结回火后的磁体继承下去,而烧结中形成的Nd2Fe14B相和B-rich相在回火后数量和形态基本上变化不大,Nd-rich相虽然数量变化也不大,但是在高温回火中熔化流动,均匀分布在主相Nd2Fe14B周围,把主相Nd2Fe14B一个个分隔开来,在低温回火中,这种流动会延续,相的形态会得到巩固,使得磁体最终获得良好的综合磁性能。     

稀土La在纳米晶（W, Ni, Fe, La）复合粉末烧结过程中的作用机理

采用溶胶-喷雾干燥法制备纳米晶(W,Ni,Fe,La)复合粉末,研究了粉末在烧结过程中La对抑制鼓泡和晶粒长大的作用机理,通过XRD与SEM分析了La在烧结过程中的相转变规律和在合金中的存在形式,讨论了稀土La对合金液相烧结过程中扩散的影响。结果表明:稀土La在纳米复合粉末中主要以La2WO6与La4W2O15的形式存在。经液相烧结后,稀土La主要以二次相颗粒的形式分布于粘结相中,生成高温下能稳定存在的La4W2O15相,该相对杂质元素Ca、O具有很好的亲和力,起到晶界净化和晶内净化的作用。同时二次相颗粒存在于粘结相中,抑制了W在粘结相中的扩散,降低了W在粘结相中的溶解度,使得液相烧结溶解-析出过程减慢,从而抑制液相烧结阶段的晶粒长大和鼓泡现象。     

PHASE COMPONENT AND CURIE TEMPERATURE OF Nd_4(Fe_(1-x)Cr_x)_(77.5)B_(18.5)ALLOYS

1.IntroductionThenewhard-magneticNdFeBall0yswithlowNdc0ncentration(35at.%)havebeenobtainedbycrystallization0fam0rphous.ibbo.sI1-3].Theirmagneticpr0pertiesatr0omtemperatureareasfollows:coercivityHc=16O-24OkA/m,remanenceB,=1'2-1.25T,andmagneticenergy(BH).ax=64108kJ/m'.ThevaluesofB.and(BH).axaremuchhigherthanth0se0fthewidelyusedanis0tropic(Ba,Sr)Fe12Ol9ferritesandAlNiC0alloys.Inpreyi0uspapers['-'1,wehavereportedthestructuralandmagneticpr0perties.Recentlywestudiedtheinfluenceofthesubstit…