Effects of milling and crystallization conditions on microstructure of Nd2Fe14B/α-Fe powder

Effects of milling and crystallization conditions on microstructure,such as amorphous phase and nanocrystalline phase, were investigated by X-ray diffractometry(XRD),differential scanning calorimetry(DSC),and transmission electron microscopy (TEM),respectively.The results show that nanocomposite Nd2Fe14B/α-Fe powder can be prepared by mechanical milling in argon atmosphere and a subsequent vacuum annealing treatment.The grain sizes of both Nd2Fe14B andα-Fe phase decrease drastically with increasing milling time.After milling for 5 h,the as-milled material consists ofα-Fe nanocomposite phases with the grain size of 10 nm,and some amorphous phases,which can be turned into Nd2Fe14B/α-Fe nanocomposite phases by the subsequent annealing treatment.Milling energy of mechanical milling after 5 h by theoretical calculation is 6 154.25 kJ/g.     

Nb对Nd2Fe14B／α-Fe纳米复合永磁材料结构和磁性能的影响

添加Nb可提高（Nd0.9Dy0.1）9.5Fe79Co5B6.5（原子百分数，下同）合金的非晶形成能力和快淬薄带的晶化温度，经过710℃晶化处理4min后，快淬薄带的晶粒细小均匀，从而显著提高了快淬薄带的磁性能。三维原子探针（Three-Dimensional Atom Probe，简称3DAP）分析结果表明，含Nb快淬薄带晶化后，在晶界形成了Nb-Fe-B偏聚物，抑制了晶粒长大，细化了晶粒，进而使晶粒间交换耦合作用增强，提高了合金的磁性能。     

添加Sn对Nd2Fe14B/α-Fe纳米复合永磁材料结构和磁性能的影响

在Nd10Fe84B6添加0.5 at%Sn元素,合金晶化后Sn富集于富Nd相,富Nd相的生成使得合金中α-Fe相的相对含量增加,合金的剩余磁化强度,矫顽力和剩磁比有所改善。而在Nd9.5Fe75.5Co5Zr3.5B6.5合金中添加1 at%Sn元素后,虽然晶化后合金的晶粒变细小,α-Fe相的相对含量也有所增加,然而由于过多的富Nd相、富B相和富Zr相等软磁性相或非磁性相的存在,使得合金的剩余磁化强度和磁滞回线的方形度降低,进而降低了合金的综合磁性能。     

快淬速度对Nd2Fe14B/α-Fe纳米复合永磁材料结构和磁性能的影响

利用熔体快淬法制备了(Nd0.9Dy0.1)9(Fe0.9Co0.1)85.5B5.5快淬薄带,研究了快淬速度对晶化过程、晶化后薄带的结构及磁性能的影响.研究发现,快淬速度不同,薄带的非晶程度不同,晶化过程存在很大差异;在快淬速度为12m/s时,快淬薄带中已存在一定的晶态相,晶化后的晶粒细小均匀,磁性能较高;而当快淬速度达到18m/s和25m/s时,合金晶化后的晶粒粗大且不均匀,磁性能较低.     

短时热处理对Nd2Fe14B/α-Fe纳米复合磁体结构和磁性影响

罗马尼亚Babes-Bolyai大学物理系V.Pop等人采用高能球磨法制得Nd2Fe14B/α-Fe纳米复合磁体,并选用700℃、750℃、800℃短时间退火,同传统的550℃×1.5h退火对比。结果发现,短时间退火更有利于硬磁相再结晶,抑制软磁相成长,     

Nd2Fe14B／α-Fe／非晶Nd-Fe-B三相纳米交换耦合磁体中的结构弛豫

用旋淬法制备了Nd2Fe14B／α-Fe基复相纳米交换耦合磁体粉末样品．发现样品由于在室温下的结构弛豫导致磁性能的较大变化．在淬态Nd-Fe-B非晶相和Nd2Fe14B／α-Fe纳米晶共存的三相交换磁体中,其效果更为明显．而在淬态完全非晶态或晶态的单相或复相交换磁体中,结构弛豫对磁性能的影响较弱．淬态Nd10Fe83B6In磁体粉末经过在室温下置放1年时间后,内禀矫顽力Hc由刚出炉时的296kA／m增加至384kA／m,剩磁比mr从0．55增至0．62．非晶相的存在为晶粒发展完备的晶界提供了可能,应力和缺陷集中的边界区域的结构弛豫和原子调整使得相邻接的相与相、晶粒与晶粒之间的结晶学相关性提高,交换耦合增强．同时完善的晶界也增强磁体的磁硬化．X射线衍射结果显示结构弛豫的最终结果使得衍射峰宽化,极有可能在晶界处形成了畸变的晶间相．而正是这种畸变的晶间相对磁性能的增强起了关键的作用。     

微合金化α-Fe/Nd2Fe14B纳米复合材料的显微结构与磁性能

微合金化是提高α-Fe/Nd2Fe14B和Fe3B/Nd2Fe14B纳米复合磁体综合磁性能的常用方法。在许多情况下，微合金化元素如铜和钕明显减小晶粒尺寸，优化硬磁性能。人们采用三维原子探针(3DAP)和透射电子显微术研究了Fe3B/Nd2Fe14B纳米复合材料微结构形成过程中铜和钕原子的团聚和偏析行为，结果发现，铜原子在非晶晶化前形成高密度原子团(~1024/m3)，这些原子团成为Fe3B初次晶的非均匀形核位置，从而细化了最终纳米复合材料的组织结构。日本筑波材料科学研究所材料工程实验室材料物理小组的D. H. Ping研究了这些微量元素在α-Fe/Nd2Fe14…     

Magnetic properties of Nd_2Fe_(14)B/α-Fe nanocomposite magnets with yttrium addition

The phase evolution and magnetic properties of Nd9?xYxFe72Ti2Zr2B15 (x = 0,0.5,1,and 2) melt-spun nanocomposite ribbons were studied.It is found that Y addition not only enhances the formability of amorphous phase in the alloy,but also stabilizes the amorphous phase during the annealing treatment.The appropriate content of Y addition effectively enhances the remanence (Jr) of the annealed sample.The residual amorphous intergranular phase in the annealed sample optimizes the squareness of the loop,resulting in an larger maximum energy product (BH)max.The best magnetic properties,Jr = 0.78 T,Hci (coercivity) = 923.4 kA/m,and (BH)max = 98.5 kJ/m3,were obtained from the Nd8YFe72Ti2Zr2B15 ribbon spun at Vs = 4 m/s and annealed at 700°C for 10 min,which is composed of Nd2Fe14B,α-Fe,and amorphous phase.     

动态晶化对纳米晶交换耦合Nd2Fe14B/α-Fe磁性能和显微组织的影响

为改善纳米晶交换耦合Nd2Fe14B/α-Fe永磁合金微结构以提高磁性能，用熔体快淬和动态晶化热处理的方法制备了纳米晶交换耦合Nd2Fe14B/α-Fe永磁体，采用XRD和TEM等方法系统研究了动态晶化热处理对Nd10.5（FeCoZr）83.4B6.1永磁体磁性能和显微组织的影响。结果表明：与传统晶化相比，动态晶化可以在相同的晶化温度下缩短晶化时间，同时能细化晶粒，增强晶粒间磁交换耦合作用，提高磁性能。Nd10.5（FeCoZr）83．4B6.1合金快淬薄带经700℃，10min动态晶化热处理后，制得的粘结磁体获得最佳磁性能，剩磁Br=0．685T，内禀矫顽力Hcj=732kA／m，磁感矫顽力Hcb=429kA／m，最大磁能积（BH）m=75kJ／m^3。     

Nd_2Fe_(14)B/α-Fe/非晶Nd-Fe-B三相纳米交换耦合磁体中的结构弛豫

用旋淬法制备了Ｎｄ２Ｆｅ１４Ｂ／α－Ｆｅ基复相纳米交换耦合磁体粉末样品．发现样品由于在室温下的结构弛豫导致磁性能的较大变化．在淬态Ｎｄ－Ｆｅ－Ｂ非晶相和Ｎｄ２Ｆｅ１４Ｂ／α－Ｆｅ纳米晶共存的三相交换磁体中,其效果更为明显．而在淬态完全非晶态或晶态的单相或复相交换磁体中,结构弛豫对磁性能的影响较弱．淬态Ｎｄ１０Ｆｅ８３Ｂ６Ｉｎ磁体粉末经过在室温下置放１年时间后,内禀矫顽力Ｈｃ由刚出炉时的２９６ｋＡ／ｍ增加至３８４ｋＡ／ｍ,剩磁比ｍｒ从０．５５增至０．６２非晶相的存在为晶粒发展完备的晶界提供了可能．应力和缺陷集中的边界区域的结构弛豫和原子调整使得相邻接的相与相、晶粒与晶粒之间的结晶学相关性提高,交换耦合增强．同时完善的晶界也增强磁体的磁硬化．Ｘ射线衍射结果显示结构弛豫的最终结果使得衍射峰宽化,极有可能在晶界处形成了畸变的晶间相．而正是这种畸变的晶间相对磁性能的增强起了关键的作用．     

两种方法制备纳米晶复相Nd2Fe14B/α-Fe永磁体实验研究

将机械球磨后制备的Nd2Fe14B非晶粉末和α-Fe纳米晶粉末分别采用2种方法制备纳米复相Nd2Fe14B/α-Fe永磁体。第1种方法是直接将其冷压制坯、真空包套和热挤压制备永磁体。第2种方法是先将Nd2Fe14B晶化,然后冷压制坯、真空包套和热挤压制备永磁体。利用TEM、VSM等分析手段对比研究了2种方法制备永磁体的相对密度、微观组织以及磁性能。结果表明:在相同的工艺参数下,第1种方法制备永磁体不仅可以减少工序,而且其制备的永磁体综合性能均优于第2种方法,其制备永磁体的相对密度为98.24%;Nd2Fe14B和α-Fe的晶粒尺寸分别为60和80nm;磁性能达到:Br=0.98T,Hci=305.6kA/m,和(BH)m=89.8kJ/m3。     

低稀土含量的纳米复相α-Fe/Nd2Fe14B淬态合金微结构与微波电磁特性研究

对低稀土含量的Nd6Fe91B3合金进行熔体快淬处理,制备了由a-Fe相和少量的Nd2Fe14B相组成的纳米复相材料,并对其进行球磨处理25 h.研究了快淬速度对淬态合金的相组成、微观结构、微波电磁性能的影响规律.研究结果表明,随着淬度的提高,淬态合金中高磁晶各向异性的Nd2Fe14B相逐渐减少,材料的自然共振频率向低频移动,但样品微波磁导率随淬速的提高而升高.淬速为40 m/s的样品微波磁导率虚部在4.17 GHz获得最大值μrmax=4.66,其实部在1.55 GHz获得最大值μmax =7.88.同时,低稀土含量的纳米复相α-Fe/Nd2Fe14B材料具有良好的微波电特性,其复介电常数在2 GHz附近出现共振.由于磁损耗和电损耗共同作用,有利于该材料在GHz频段电磁波吸收材料中的应用.     

Crystallization behaviour and high coercivity of （Nd,Pr）（13）Fe（80）Nb1B6 melt-spun ribbons

Amorphous (Nd,Pr)₁₃Fe₈₀Nb₁B₆ ribbons were crystallized at 670–730°C for 5–25 min to study the effects of isothermal crystallization on their behavior and magnetic properties. XRD results indicate that the isothermal incubation time is 12, 5, and less than 5 min at 670, 700, and 730°C, respectively. High coercivities, with the maximum value of _i H _c = 1616 kA/m at 700°C for 19 min, measured by a physical property measurement system, are obtained in the crystallized ribbons. This is mainly attributed to the addition of Pr and Nb, because Pr₂Fe₁₄B has a higher anisotropic field than Nd₂Fe₁₄B, and Nb enriched in the grain boundary regions can not only reduce the exchange-coupling effects among hard grains, but also impede grain growth during the crystallization process. In addition, it should also be related to the characteristics of the furnace that the authors designed.     

粉末热挤压制备纳米晶复相Nd2Fe14B/α-Fe永磁体

将球磨后获得的Nd2Fe14B非晶相和α-Fe纳米晶直接进行冷压制坯、真空包套、粉末热挤压来制备近致密的纳米晶复相Nd2Fe14B/α-Fe永磁体.借助于X射线衍射(XRD)、透射电子显微镜(TEM)和振动样品磁强计(VSM)等分析方法研究了挤压温度为950℃时,不同加热时间磁体相对密度、微观组织和磁性能的影响规律.结果表明,随加热时间的延长,Nd2Fe14B及α-Fe的晶粒尺寸逐渐长大.当挤压温度为950℃,加热时间为15 min时,Nd2Fe14B及α-Fe的晶粒尺寸比较细小,分别为60和80 nm,此时磁性能最好,达到Br=0.98T,Hci=305.6 kA/m和(BH)m=89.8kJ/m3.     

Crystallization behaviour and high coercivity of （Nd,Pr）（13）Fe（80）Nb1B6 melt-spun ribbons

Amorphous (Nd,Pr)13Fe80Nb1B6 ribbons were crystallized at 670-730℃ for 5-25 min to study the effects of isothermal crystallization on their behavior and magnetic properties. XRD results indicate that the isothermal incubation time is 12, 5, and less than 5 min at 670, 700, and 730℃, respectively. High eoercivities, with the maximum value of iHc = 1616 kA/m at 700℃ for 19 min, measured by a physical measurement system, are obtained in the crystallized ribbons. This is mainly attributed to the addition of Pr and Nb, because Pr2Fe14B has a higher anisotropic field than Nd2Fe14B, and Nb enriched in the grain boundary regions can not only reduce the exchange-coupling effects among hard grains, but also impede grain growth during the crystallization process. In addition, it should also be related to the characteristics of the furnace that the authors designed.     

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。