烧结Nd-Fe-B磁体的温度稳定性缺陷分析

采用SEM、EDAX及粒度分析手段,研究了烧结Nd-Fe-B磁体开路磁通不可逆损失(hirr)异常偏高的原因。结果表明,磁体显微组织中晶粒尺寸分布不均匀及存在少量粗大晶粒,是导致其温度稳定性缺陷的主要因素,表现为少数产品hirr异常偏高。在磁体工业生产过程中,改进原料的铸锭和制粉技术,避免出现粗大粉末颗粒,减少极细粉末颗粒的数量,保证磁体显微组织精细均匀,是制备温度稳定性高的烧结Nd-Fe-B磁体的基本措施。     

Al与Mo复合添加对NdFeB磁体矫顽力的影响

本文采用晶间合金化工艺将合金元素Mo和Al直接引入烧结Nd-Fe-B磁体晶间区域,改变晶间区域的合金体系和显微组织,以达到提高磁体矫顽力的目的.实验结果表明Mo在低温时效过程中可抑制晶间富Nd相与主相之间的平衡转变,使晶界区域析出细小二次主相晶粒,使矫顽力提高.     

废弃Nd-Fe-B磁体的回收技术研究

在制备烧结Nd-Fe-B的过程中加入少量废弃Nd-Fe-B磁体,并相应减少Nd、Fe、B原料的投料量,再经过成形、烧结和后加工工序制成样品;对含废料与不含废料的Nd-Fe-B样品的粉末粒度、微观结构和磁性能进行了测试和比较分析。结果显示,含废料样品的粒度集中性略低于不含废料样品,且有少部分颗粒粒径超过100μm,而二者的微观结构基本一致,且随着老化温度升高,磁通量均有所减小,热变化规律相同。     

Fe基多孔材料瞬时液相烧结过程研究

采用定量DSC差热分析、扫描电镜分析、背散射元素分析以及XRD物相分析等方法对添加Ni-P共晶合金的Fe粉瞬时液相烧结过程进行了研究.研究发现,粉末颗粒粒度、烧结时间等参数对烧结过程有重要的影响.粉末粒度较小时,烧结升温过程中元素间的固相扩散比较明显,但粉末粒度对形成液相的总量影响较小.液相烧结时,固相Fe元素向液相中...     

烧结温度对Nd24.38Ce0.52Gd6.65Febal.TM1.76B0.95磁体组织与性能的影响

采用双合金法制备Nd24.38Ce0.52Gd6.65Febal.TM1.76B0.95（质量分数,%）永磁体,通过扫描电镜及能谱、AMT-4磁测试仪、电子万能力学试验机等手段研究烧结温度对磁体组织和性能的影响.结果表明：随烧结温度从1060℃升高到1100℃,在烧结温度为1080℃时,晶粒均匀且结合致密,富稀土相分布均匀,能获得较好的组织形态;富稀土相中稀土总含量从84.98%增加到98.04%,烧结过程中铈从主相显著扩散到富稀土相;磁体剩磁Br、矫顽力Hcj、磁能积（BH）max 先升后降,在1080℃烧结时获得较好的磁性能,分别为1.22 T、964 kA/m 和293 kJ/m3,同时磁体抗弯强度也达到最大值为257 MPa.     

生坯密度对烧结 Nd-Fe-B 磁体结构与性能的影响

结合国内烧结Nd-Fe-B磁体工业生产过程，研究了压制成型时生坯密度变化对烧结Nd—Fe—B磁体致密化程度、显微组织、取向度与磁性能的影响。试验结果表明，生坯密度的提高可促进烧结致密化过程，抑制烧结过程晶粒的不均匀长大，提高取向度，改善磁性能。     

废旧烧结Nd-Fe-B磁体添加Ce再制造技术研究

烧结Nd-Fe-B磁体再生过程中会引起稀土元素的氧化和损失,因此重新烧结时无法致密化。添加Ce金属,有助于再生磁体的致密化,并优化磁体的显微组织结构。通过低成本Ce金属的添加,成功实现再生磁体的综合性能优化。并研究了废旧烧结Nd-Fe-B磁体的吸氢过程,用BH测试仪测试了再生磁体的磁性能;采用扫描电镜观察了再生磁体的微观结构。添加4%Ce(质量分数)时,在1 350 K烧结、773 K热处理条件下,再生磁体的剩磁达到了原磁体的98%以上,内禀矫顽力超过了原磁体。     

无重稀土烧结Nd-Fe-B磁体的显微结构和磁性能研究

对Ga、Al、Cu和Zr共同掺杂的烧结Nd-Fe-B磁体磁性能和显微结构进行研究，并通过回火工艺对磁体的矫顽力进行调控。结果表明：当一级回火为900℃×150 min,且二级回火为500℃×180 min时，磁体矫顽力H_cj从烧结态的14.33 kOe大幅提高到二级回火态的19.86 kOe,提高了38.6%;方形度H_k/H_cj由0.86增加到0.97;剩磁B_r仅从烧结态13.51 kGs略微下降到二级回火态的13.46 kGs;富稀土相分布更加连续和明显。研究分析表明，矫顽力大幅增加主要是由于含有少量的富Nd相和贫B相的烧结Nd-Fe-B磁体中Ga的掺杂改变了晶界相湿润性，降低了富稀土相中Fe元素的含量。本研究为无重稀土高矫顽力和高剩磁烧结Nd-Fe-B磁体步入产业化夯实了理论基础。     

添加Dy、Nb对烧结NdFeB磁体结构与性能的影响

采用SC工艺制备了Nd-Fe-B合金铸片,研究了在合金铸片中添加Dy、Nb元素对合金铸片显微结构和烧结Nd-Fe-B磁体磁性能的影响,确定了Nd-Fe-B磁体获得最佳磁性能时Dy元素、Nb元素的含量,并用扫描电镜、磁性能测量仪等对其进行了分析和测量。实验结果表明,Dy元素的添加可以使晶粒细小化、均匀化、规则化,在不显著影响剩磁的情况下大幅度提高磁体的内禀矫顽力;在含Dy元素和Co元素的磁体中加入少量Nb元素可以在不显著影响剩磁的情况下较大幅度提高磁体的内禀矫顽力,降低磁通不可逆损失,提高磁体使用温度。     

超固相线液相烧结GH4049粉末合金

采用超固相线液相烧结方法制备了GH4049粉末合金,研究了合金的致密化机理、热处理对合金组织和力学性能的影响以及Y2O3对合金的强化作用.结果表明:在1 350 ℃真空烧结120 min可以制备出相对密度为99.2%的GH4049粉末合金,合金的烧结致密化机理为颗粒重排与粘性流动.经热处理后,GH4049粉末合金的抗拉强度、屈服强度和伸长率分别为1 113 MPa、760 MPa和13%,接近变形GH4049合金;晶内析出了约200 nm的方形大γ'相和40 nm左右的球形γ'相,平均晶粒大小在80 μm以下.加入质量分数为0.05%的纳米级Y2O3后,改善了合金的抗应力松弛性能.     

Grain Growth Behavior in Sintered Nd-Fe-B Magnets

The Nd2Fe14B grain growth behavior in sintered Nd-Fe-B magnets was quantitatively described.The effects of sintering temperature and time,and alloy powder size and its distribution on grain growth process were analyzed.Hence,possible grain growth mechanisms in these magnets were qualitatively discussed.The Nd2Fe14B grain growth proceeded at quite a high rate in the initial 0~1 h of sintering and from then onwards the grain growth rate decreased.A large average particle size or a wide particle size distribution of initial alloy powders was found to remarkably accelerate the grain growth process and even result in the occurrence of abnormal grain growth.On the basis of experimental results,two grain growth mechanisms were considered to operate during sintering of Nd-Fe-B magnets,that is,dissolution and re-precipitation of Nd2Fe14B particles,and Nd2Fe14B particle growth by coalescence.It was believed that Nd2Fe14B particle growth by coalescence not only produced a large average grain size and a wide grain size distribution,but also was the fundamental reason for the formation of abnormally large grains in the microstructure of sintered Nd-Fe-B magnets.     

Effects of Pr-Cu-Ti intergranular addition on microstructure and magnetic properties of heavy-rare-earth-free Nd-Fe-B sintered magnets

By intergranular addition of Pr-Cu-Ti alloy powders in the Nd-Fe-B sintered magnets with the normal B component, we propose an approach to the optimization of grain boundary and local Nd-Fe-B composition system. The coercivity is enhanced from 1.42 to 1.86 T, while further addition leads to a reduction in remanence and coercivity. The analyses of phase composition reveal that Ti mainly exists in the form of metallic Ti alloy, and part of Ti combines with B to form the TiB₂ phase after the liquid phase sintering process. This process results in a consumption of B in the local Nd-Fe-B composition system and a change of the grain boundary component, which contributes to the formation process of the RE₆(Fe,M)₁₄ phase after the annealing process. Therefore, with the modification of grain boundary and composition system, the intergranular addition of Pr-Cu-Ti induces the generation of continuous thin grain boundary phases. It promotes the intergrain exchange decoupling, increasing the coercivity in the annealed magnet. While the excess addition results in the segregation of TiB₂, as well as the precipitation of TiB₂ into the Nd-Fe-B phase, which leads to structural defects. Thus, the further effort for the addition alloy with Ti to reduce the deterioration of the microstructure will lead to further improvement in magnetic properties.     

Spark Plasma Sintering Nd-Fe-B Permanent Magnets With Good All-Around Property

In present study, sintered Nd-Fe-B permanent magnets with different compositions were fabricated by using both Spark Plasma Sintering (SPS) technique and conventional sintering technique. Microstructure and compositions of both magnets are observed by scanning electron microscope with energy dispersive X-ray detector. Magnetic properties, mechanical properties, and chemical stabilities of both Nd-Fe-B magnets are investigated. Compared with the conventional sintered magnets, SPS Nd-Fe-B magnets possess comparable magnetic properties, better corrosion resistance and mechanical properties. Further investigation shows that the good all-around properties of the SPS magnets result from their unique microstructure. In detail, the grain size of Nd₂Fe₁₄B main phase is fine and uniform, only a few Nd-rich phase forms along the grain boundaries of Nd₂Fe₁₄B, while most of them agglomerates into the triple junctions. As a result, SPS process is expected to be a promising method for the production of new Nd-Fe-B magnets with good all-around properties.     

Spark-Plasma Sintering of W-5.6Ni-1.4Fe Heavy Alloys: Densification and Grain Growth

W-5.6Ni-1.4Fe heavy alloys were prepared by the method of spark-plasma sintering, and the densification and grain growth kinetics were analyzed as a function of various parameters such as sintering temperature and dwell duration. It is found that the local temperature gradient at the vicinity of the pores can cause the matrix phase melting or softening, resulting in a viscous layer coating the W particles and an improved solubility of W into the matrix phase. In the initial stage, particle rearrangement and neck formation and growth take place, and γ-(Ni, Fe) matrix phase has formed. Dissolution-precipitation and Ni-enhanced W grain boundary diffusion together with viscous process contribute to the simultaneous densification and grain growth in the intermediate stage. During the final stage, fast grain growth, controlled by both gas-phase diffusion and dissolution-precipitation mechanisms, dominates over the densification.     

烧结Nd-Fe-B磁体晶界扩散TbH2高温稳定性及其机理

采用涂敷方式,在烧结钕铁硼表面均匀涂敷TbH₂粉末,经过不同的扩散温度处理,制备出晶界扩散磁体。研究了晶界扩散TbH₂对烧结Nd-Fe-B磁体常温磁性能及高温稳定性的影响,并分析了磁体矫顽力提升的机理。常温磁性能研究表明,扩散磁体经过890 ℃+490 ℃工艺处理后性能达到最优,矫顽力从1 383 kA/m提升到1 988 kA/m。高温磁性能结果显示,扩散磁体200 ℃的矫顽力温度系数|β|比原始磁体降低0.032%/℃,磁通不可损失hirr比原始磁体降低21.47%,扩散TbH₂明显提高了烧结Nd-Fe-B磁体的热稳定性。分析得出,晶界扩散TbH₂磁体矫顽力提升的机理是Nd₂Fe₁₄B晶粒外延层形成了（Tb, Nd）₂Fe₁₄B核壳结构,提高了磁晶各向异性场;同时改善了磁体的微观组织结构,有效地隔绝了晶粒之间的磁交换耦合作用。      

成形压力对烧结Nd-Fe-B磁体微观组织与磁性能的影响

在于法制备烧结钕铁硼生产线上,研究了11.54 MPa和9.23 MPa两种成形压力对Φ9.5mm烧结钕铁硼磁体(/%:31.00Pr+Nd、1.20B、0.20Al、余Fe)微观组织与磁性能的影响。结果表明,成形压力增大可以改善晶粒分布的不均匀性,提高取向度,从而提高剩磁与磁能积;但成形压力增大易使晶粒尺寸增大,从而使矫顽力降低。     

烧结钕铁硼的微观结构研究

利用扫描电镜观察了35AH、N35、N50和33SH四个牌号不同尺寸长方体形的烧结Nd-Fe-B磁体的微观结构。从晶粒的大小、形状、分布和晶界状况等方面比较了高性能与普通性能烧结Nd-Fe-B磁体微观结构的异同。高性能磁体的微观结构更接近于理想状态，即主相晶粒细小，分布均匀，形状规则，有适量的呈薄层状分布的富钕相将主相晶粒包裹。     

Microstructure and Magnetic Properties of Anisotropic Nd-Fe-B Magnets Fabricated by Single-Stage Hot Deformation

Anisotropic Nd-Fe-B magnets were fabricated by the single stage hot deformation (SSHD) method. The magnetic properties of the anisotropic Nd-Fe-B magnets are as follows: the maximum energy product is 234.7 kJ·m-3, remanence 1.16 T and coercivity 684.3 kA·m-1. A study of the relationship between microstructure and magnetic properties for the anisotropic Nd-Fe-B magnets was carried out. The results show that the grains of Nd2Fe14B have grown up preferentially along the direction perpendicular to the pressing direction.     

Determination of pore mobility during sintering

The mobility of pores being dragged by grain boundaries has been modeled in terms of shape-independent microstructural parameters measurable by stereological means. The derived mobility is expressed with respect to the amount of porosity per unit area of grain boundary and the driving pressure for grain boundary and pore motion,i.e., as velocity per unit driving pressure. The resultant mobility for pore surface diffusion-controlled motion is found to be inversely proportional to the mean-pore intercept, regardless of pore shape and volume fraction. Solutions for lattice and vapor transport yield mobilities independent of pore size but inversely proportional to pore volume fraction. Computed pore mobilities, assuming surface diffusion-controlled motion, during final-stage sintering of copper and tungsten are shown to decrease with densification. In one case, mobility was found to increase during early densification, prior to the final stage. These results are explained with reference to the simultaneous changes occurring in grain boundary and pore surface areas during densification.