DESIGN AND PREPARATION OF IN SITU Pb-RICH PARTICLES/Al BASE METALLIC GLASS MATRIX COMPOSITE

在Al--Pb二元难混溶合金的基础上添加其它的合金元素Ni, Y和Co, 优化设计了新的 Al_82.87Pb_2.5Ni_4.88Y_7.8Co_1.95多元难混溶合金. 开展了该多元难混溶合金的快速凝固实验, 对制备的薄带样品进行了结构表征、热稳定性分析以及显微组织形成的研究. 结果表明, 合金熔体在快速冷却过程中发生了液-液相分离, 生成富Al和富Pb两液相; 随后, 富Al基体液相发生玻璃转变, 形成铝基非晶合金基体, 而富 Pb液相凝固结晶后以球形晶态粒子形式均匀分布于铝基非晶基体中. 研究表明, 利用难混溶合金液-液相变原理, 通过快速凝固技术可以设计和制备原位球晶粒子/非晶合金基复合材料.     

双主相混合稀土基RE-Fe-B磁体的磁性能和抗腐蚀性改进

为了实现稀土资源的平衡应用且降低RE-Fe-B稀土永磁材料的价格,针对混合稀土基永磁材料进行研究,分别采用单、双主相工艺制备了名义成分[(Pr,Nd)_1-xMM_x]_30.3(Fe,Co)_balM_0.73B_0.98 （x=0.3,0.5和0.7,质量分数）的磁体,对比研究其磁性能和抗腐蚀性。研究发现：双主相工艺制备的磁体相比单主相工艺制备的同成分磁体展现了优越的磁性能和抗腐蚀性。当x=0.5,双主相磁体的磁性能为B_r=1.308 T,H_cj=799.98 kA/m和(BH)_max=325.6436 kJ/m³,远高于同成分的单主相磁体的性能（B_r=1.297 T,H_cj=746.8868 kA/m 和(BH)_max=317.8428 kJ/m³）。这种改进源于富稀土相分布的改进以及主相晶粒间和晶粒内部耦合作用的增强。当双主相磁体暴露在湿热环境下时,磁体中不仅存在富稀土相腐蚀,也存在主相晶粒的腐蚀成粉现象,这主要是由于富稀土相与水蒸气和氧气反应时产生氢气,导致主相晶粒被氢化,由于主相晶粒间和晶粒内部的镧铈分布差异,产生大的应力,导致其表现出区别于单主相磁体的腐蚀行为。     

典型Cu-Ni-P合金体系物相提取合成多孔结构Ni-P颗粒

基于不同Ni、P原子比设计合成了Cu-Ni-P系列合金，并针对其特有的微观组织及物相提取过程进行了研究。研究发现，Cu-xNi-4.5P合金铸锭内含有Cu和多种Ni-P物相，如Ni₅P₄、Ni₁₂P₅及Ni₃P。经过熔体旋淬处理后，其薄带试样中磷化物主要以Ni₁₂P₅和Ni₃P形式存在。此外，对比发现，合金内镍含量的增加在一定程度上促使了磷化物相的粗化。通过调控合金的凝固行为及物相提取工艺，可获得多级孔结构的Ni-P颗粒，其孔洞是由于腐蚀过程中铜基体、共晶组织内及固溶部分的铜被去除而形成的。通过对典型合金进行物相提取，实现了可控合成磷化物，这对于拓展功能性磷化物的应用具有促进作用。     

微束等离子弧熔化沉积TiAl/Ti2AlNb梯度材料的组织与相变

采用微束弧热态焊技术熔化沉积Ti₂AlNb合金丝材,在TiAl基合金环状试样上制备出Ti₂AlNb基合金梯度材料。利用金相显微镜(OM)、扫描电子显微镜(SEM)、能谱分析(EDS)、X射线衍射(XRD)方法及显微硬度测试,对沉积态TiAl/Ti₂AlNb梯度材料的显微组织、相组成和显微硬度进行了分析。结果表明：微束弧热态焊技术熔化沉积的Ti₂AlNb基合金组织由β相、O相和α₂相组成,并且随着距离母材距离的增加,梯度材料呈现出γ+α₂/γ→β(固溶体)+O→β₂+O+α₂(魏氏组织)→β(固溶体)+O的相变趋势。梯度材料的硬度呈现出波浪式的分布。另外结合各元素对组织稳定性的影响,以及微束等离子技术所具有的特殊热循环和热积累效应,对梯度材料在微束等离子沉积过程中的相变规律进行了解释。     

Nd2Fe14B/α-Fe永磁材料中软磁相晶粒尺寸及其含量的确定

在前人对Nd₂Fe₁₄B/α-Fe永磁材料中软磁相晶粒尺寸及其含量的实验结果和分析的基础上,通过建立简单模型进一步证明并相对精确的计算了双相纳米复合永磁材料中软磁相晶粒尺寸及软磁相的含量范围。综合分析得出Nd₂Fe₁₄B/α-Fe永磁材料获得最优磁性能时的软磁相尺寸~8nm,软磁相含量~40%。该数据为FePt / Fe₃O₄和Sm₂Fe₁₇N₃/α-Fe等其它双相纳米复合永磁材料最有磁性能对晶粒尺寸及其含量的要求在理论上奠定了基础。     

综述：Ti-Al反应扩散机理及动力学(下)

通过Ti和Al制备的Ti-Al系金属间化合物及复合材料由于具有优异的物理、化学和力学性能,在航空航天、汽车以及其它领域具有良好的应用前景。这些材料包括TiAl₃、γ-TiAl和α₂-Ti₃Al等金属间化合物,以及Ti/Al、Ti/α₂-Ti₃Al、Ti/γ-TiAl、Ti/TiAl₃、Ti/TiAl₃/Al和Al/TiAl₃等金属-金属或金属-金属间化合物复合材料。在上述材料的制备过程中,会涉及到各种Ti-Al反应扩散过程。因此,对Ti-Al反应扩散机理及动力学的深入理解,有助于合理高效的制备Ti-Al系金属间化合物及复合材料。目前对Ti-Al反应扩散机理及动力学的研究非常广泛,但很多结论仍存在争议。本文(下)部分系统综述了Ti-Al反应扩散动力学的研究现状,并对其未来的研究方向进行了展望。     

一种新型经济高效非晶涂层的制备与性能表征

利用火焰喷涂技术喷涂自制的气雾化合金粉末取代非晶粉末,制备了NiFeBSiNb非晶纳米晶涂层。分别对粉末和涂层的微观组织结构和热力学性能进行了表征。结果表明,自制的合金粉末球形度较好,大多为球形或椭球形;主要为晶体结构,由Nb₂Ni₂₁B₆晶体相和(Ni,Fe)₂₃B₆固溶体组成。而经过火焰喷涂制备的涂层,形成了非晶相和纳米晶相。通过公式计算此合金体系粉末和涂层形成非晶相的临界冷却速率分别为6.01×10₅K/s和4.56×10₃K/s,解释了在粉末制备过程中较难形成非晶相而喷涂过程中形成非晶结构比较容易。对涂层的摩擦磨损性能进行了测试,涂层摩擦系数仅为0.17,具有优异的耐磨性能。     

激光增材制造Ti6Al4V-Inconel718功能梯度材料的成分变化和微观结构演变

利用激光增材制造技术制备了Ti6Al4V/Inconel718功能梯度材料,研究了该梯度材料的成分及相组成、显微组织和显微硬度的变化。研究表明：沿组成梯度方向发生了一系列相变：α+β→α+β+Ti₂Ni→β+TiNi→γ,过渡层主要是由TiNi和Ti₂Ni以及Ti-Cr和Ti-Fe等二元相组成的混合体;沿材料底部至顶部微观组织发生了由魏氏α片层组织到细小树枝晶的转变;对沉积结构进行显微硬度测试,发现具有较高Ti₂Ni相面积分数的过渡层最硬,本研究发现最大值为823HV。     

快淬参数对Nd9.5Fe84B6.5合金磁性能和微观结构的影响

本文采用直接快淬法制备了Nd_9.5Fe₈₄B_6.5合金,研究了腔室压力和甩带速度这两个快淬参数对其磁性能和微观结构的影响,建立了两者之间的关联性。研究发现：熔体快淬过程中在其它条件保持不变时,腔室压力和甩带速度之间存在着互相补偿的关系。腔室压力为0.03 MPa、快淬速度为19 m/s时制备的条带样品与腔室压力为0.05 MPa、快淬速度为15 m/s时制备的样品厚度和磁性能的数值相近。X 射线衍射和透射电子显微镜的结果表明：这两种条件下得到的条带样品具有相同的相组成和相似的微观结构。因此,通过调整腔室压力和甩带速度可以得到微观结构和磁性能相近的条带样品,这将为制备高性能的稀土永磁材料及其工业化生产提供指导。     

Ti掺杂VO2(M)粉体制备及性能研究

M相二氧化钒(VO₂(M))是一种在68℃左右具有特殊相变特性的智能隔热窗材料,然而VO₂(M)的相变稳定性还较差、对太阳光的调制能力还不够高,严重限制其在智能隔热窗中的工业化应用。本文主要以五氧化二钒为钒源,草酸为还原剂,尿素为沉淀剂,硫酸钛为掺杂剂,水热还原法制备粉体M相钛(Ti)掺杂VO₂,简称Ti-VO₂(M)粉体。通过X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)、紫外-可见-近红外分光光度计(UV-Vis-NIR)、差示扫描量热仪(DSC)和X射线能谱仪(EDS)分析所合成粉体的元素/物相组成和结构、结晶形态、太阳光反射率/透过率和相变温度的变化情况,优化Ti^₄₊掺杂量。研究发现,Ti^₄₊掺杂量控制在3%时,制备的Ti-VO₂(M)粉体的综合性能最优,为进一步应用智能隔热有机玻璃提供重要的数据与技术支撑。     

烧结钕铁硼基底成分对晶界扩散效果的影响研究

晶界扩散作为一种能明显提升烧结钕铁硼磁体矫顽力同时实现对重稀土高质化利用的方法,日益成为目前稀土永磁学界和产业界的研究热点。本文利用自动化喷涂设备系统研究了晶界扩散烧结磁体批量制备过程中基底成分差异晶界扩散后磁体磁性能的影响,微观结构和EDS元素分析结果表明：晶界扩散后磁体矫顽力增长幅度的差异,同扩散后磁体内晶粒核壳结构形成充分与否、晶界相均匀分布与否和晶界相铁磁性元素含量高低有密切关联,同时利用晶界扩散工艺制备得到的磁体温度系数要优于传统工艺制备得到的相近似牌号的磁体。     

Microstructure and phase transformations in a liquid immiscible Fe60Cu20P10Si5B5 alloy

This work presents a study of the microstructure formed in a liquid immiscible Fe₆₀Cu₂₀P₁₀Si₅B₅ alloy during moderate cooling on a copper plate and melt-spinning. The alloy ingot was re-melted on a copper plate and observed while cooling using a mid-wave infra-red (MWIR) camera. The heating and cooling characteristics of the melt-spun ribbon were studied using differential scanning calorimetry (DSC). The morphology and chemical composition of the ingot as well as the melt-spun ribbon were analyzed using scanning electron microscopy (SEM) and energy dispersive spectrometry (EDS). The compositions of the ingot and the ribbon were investigated using X-ray diffraction (XRD). Mössbauer spectroscopic measurements showing the influence of adding Cu to the Fe–Si–P–B alloy were also analyzed.The IR images from the MWIR camera enabled direct observation and identification of the liquid state transformations of the alloy. The DSC trace of the melt-spun ribbon showed crystallization of the amorphous matrix and confirmed that high temperature transformations occurred when the alloy was in the liquid state. Observations of the microstructure of the ingot revealed crystalline surface fractal structures formed by the Fe-rich eutectic constituent and Cu-rich fcc spherical precipitates. The morphology of the precipitates indicated that the precipitates formed in the miscibility gap. The microstructure of the melt-spun ribbon is composed of an amorphous Fe-rich matrix and elongated Cu-rich fcc precipitates. The observations based on the study of the microstructure are supported by Mössbauer spectroscopy.     

Effect of annealing and heating/cooling rate on the transformation temperatures of NiFeGa alloy

In this work, Ni₅₅Fe₁₈Ga₂₇ ferromagnetic shape memory alloy was prepared through a suck-casting method. The effects of annealing and heating/cooling rate on the martensitic transformation temperatures were investigated by differential scanning calorimetry (DSC). The results showed that the phase transformation temperatures increase with increasing the annealing temperature, upon the heating and cooling process. However, the start and the finish temperatures (M_s and M_f) of martensitic phase transformation increased firstly and then decreased upon the cooling process with the increase the annealing time at 300 °C. The start and the finish temperatures (A_s and A_f) of inverse phase transformation increased slightly upon the heating process with the increase of the annealing time. The results can be explained by the evolution of the microstructure after heat treatment. It was also found that the phase temperatures show great dependence on the heating/cooling rate of the DSC test, A_s and A_f increased and M_s and M_f decreased with the increase of the heating/cooling rate.     

电子探针在钕铁硼磁性材料表征中的应用

钕铁硼稀土永磁材料在新能源汽车等行业的电机领域中应用十分广泛.使用岛津电子探针波谱仪的点分析、线分析和面分析功能对钕铁硼磁性材料微区的基体相微观特征、化学组成和分布以及晶界扩散以提高矫顽力的工艺方法进行了直观地表征,可为磁体制备新技术和微观机理的阐述提供数据参考,对生产工艺的技术改进、质量管理和失效分析等整个过程可予以...     

电子探针在钕铁硼磁性材料表征中的应用

钕铁硼稀土永磁材料在新能源汽车等行业的电机领域中应用十分广泛。使用岛津电子探针波谱仪的点分析、线分析和面分析功能对钕铁硼磁性材料微区的基体相微观特征、化学组成和分布以及晶界扩散以提高矫顽力的工艺方法进行了直观地表征，可为磁体制备新技术和微观机理的阐述提供数据参考，对生产工艺的技术改进、质量管理和失效分析等整个过程可予以有效科学指导。     

Permanent magnet materials—developments during the last 18 months

Recent permanent magnet research is largely concentrated on iron-rare earth alloys, with a large fraction dealing with the effects of alloying elements on magnets based on Fe₁₄Nd₂B. The magnetically hard phase that produced outstanding coercivities (>50 kOe) and referred to as Fe₇₀Sm₂₀Ti₁₀ in mechanically alloyed and in rapidly solidified materials turns out to be Fe₁₇RE₅ (RE = rare earth), which, in Fe-Nd alloys, is not hard at all. Work on the phases with the Mn₁₂Th structure has been only moderately successful, producing reasonably high coercivities (～10 kOe) in Fe-Sm-Ti and in melt-spun or mechanically alloyed materials, but not in sintered magnets. New iron-rare earth alloys based on Fe₁₇Nd₂N and promising higher Curie temperatures than Fe-Nd-B come as a surprise and may eventually compete with Fe-Nd-B.     

Suppression of γ phase in Ni38Co12Mn41Sn9 alloy by melt spinning and its effect on martensitic transformation and magnetic properties

Microstructure, martensitic transformation and magnetic properties of melt-spun Ni₃₈Co₁₂Mn₄₁Sn₉ ribbon were investigated and compared with its bulk counterpart. The formation of second phase (γ phase) was prevented by melt spinning. Ni₃₈Co₁₂Mn₄₁Sn₉ ribbon underwent a thermoelastic martensitic transformation at a little higher temperature than the master alloy. Due to the disappearance of γ phase, the magnetic properties of as-spun ribbon in the plane was close to its bulk counterpart. A magnetic-field-induced reverse martensitic transformation was verified in this ribbon under a relatively low magnetic field of 1.5 T. In addition, the kinetic arrest behavior was also observed even though there still existed a forward martensitic transformation when applying a magnetic field of 8 T.     

Permanent magnet materials—Developments during the past 12 months

Information about real and potential permanent magnet materials continues to grow at a rapid pace, and developments in the following areas are discussed. Co- Zr, although not comparable to the best high-performance magnets, has attracted interest as a rare earth free alloy. Carbon and nitrogen are becoming more prominent as the metalloid in iron- rare earth magnets. This leads to cast magnets based on Fe-Nd-C, bonded magnets based on Fe₁₇Sm₂N_x, a renewed interest in the tetragonal phase (Fe,Ti)_12Nd, now with added nitrogen, and a nitrogen treatment for sintered Fe₁₄Nd₂B that raises the Curie temperature by more than 100 K. Alloying additions to Fe₁₄Nd₂B improve the coercivity. Finally, developments in corrosion protection and processing are highlighted. This article was presented at the ASM Symposium on Soft and Hard Magnetic Materials, which was held 23 Oct at the combined 1991 ASM Materials Week and TMS Fall Meeting in Cincinnati, Ohio.     

U-Rh体系非晶合金的成分设计与形成特性

为了进一步认识U合金体系的非晶形成规律,本文探究了U-Rh体系的非晶形成特性。在富U端共晶区65～80 at.% U范围内设计了系列U-Rh合金,通过真空电弧熔炼制备母锭样品与甩带技术制备条带样品,采用X射线衍射和热分析手段研究了两种样品的相组成与热行为。发现U₇₀Rh₃₀合金在急冷凝固条件下形成了部分非晶相,晶化温度为642K,晶化激活能接近200kJ/mol,与之共生的是g-U高温固溶体相,这是U基非晶合金通过急冷冻结高温U固溶体的首次证据,反映出U-Rh合金非平衡凝固相变行为的独特性。结果表明,U-Rh是一个新的铀基非晶合金体系,其非晶形成能力不强,这很可能与g-U高温固溶体能被急冷直接捕获有关。     

Ce 盐封孔对 SiCp/ Al 复合材料表面 Ni-P 镀层的影响

为提高SiCp/Al复合材料的耐腐蚀性能,先化学镀镍,再沉积稀土封孔,讨论了稀土溶液主盐Ce(NO3)3浓度和沉积时间对镍-稀土多层膜耐蚀性能的影响。结果表明:化学镀镍的SiCp/Al复合材料在室温下沉积稀土时,采用Ce(NO3)3含量1 g/L、成膜时间2 h的条件获得的多层膜耐蚀性最好,其腐蚀电位为-0.48mV,腐蚀电流密度为3.54×10-8A/cm2;稀土在膜层中以Ce的氧化物颗粒堆积状态存在,起到了封孔的作用;膜层中的镍磷合金呈多晶态,而稀土含量少,未能测出;稀土溶液浓度越高,沉积速度越快,而在相同浓度下,膜层厚度随着时间的延长而增加,越厚则膜层结合力越差。