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。     

高Dy含量烧结Nd-Fe-B的晶界扩散处理研究

研究了晶界扩散处理对高Dy含量烧结Nd-Fe-B磁体性能和结构的影响。经蒸镀渗Dy晶界扩散处理,高Dy含量Nd-Fe-B磁体的矫顽力从1 713 kA/m提高至2 161 kA/m,而剩磁和最大磁能积基本没有下降,处理后磁体内Dy平均质量分数仅增加0.30%。不同深度片层分析表明,虽然磁体近表面片层比中心片层的Dy含量高,但是片层间矫顽力相差较少,而且所有片层的矫顽力均远高于未处理磁体片层的矫顽力。电子探针Dy元素面分布结果显示,在未处理高Dy含量磁体的晶界与主相中均存在Dy元素富集区且富集浓度较低,而经扩散处理后,晶界富Nd相中的Dy富集区浓度及所占比例明显提高;包括磁体芯部在内,磁体内大部分角隅处富Nd相内Dy含量明显增加,进一步提高了高Dy含量磁体内部各处的矫顽力。     

微量添加晶界合金对烧结Nd-Fe-B力学性能及微观结构的影响

采用双合金法制备系列烧结Nd—Fe—B磁体(保持其主合金成分不变：Ndl4．1Dy0．5Fe79.0B6.4(原子分数)，所添加的晶界合金中的B含量从0．95％(原子分数)逐步增加到6．95％(原子分数))，研究了微量添加晶界合金对烧结Nd—Fe—B力学性能及微观结构的影响。研究结果表明：微量添加晶界合金所制备的磁体，其抗弯强度值普遍高于单合金法制得的磁体；前者的抗弯强度最高可达397MPa，高于铸造，热压磁体的抗弯值，而后者的抗弯强度仅为309MPa。由相结构分析可知，当添加的晶界合金中的B含量为O．95(原子分数)，主相晶格的四方度减小，这时磁体具有最高的抗弯强度。另外，微量添加晶界合金，可使磁体中晶界相的分布更加均匀，从而基本上消除了主相晶粒直接接触的现象，使晶粒的不规则长大得到抑制。这也是微量添加晶界合金后磁体具有较高抗弯强度的原因之一。对磁性能的研究结果表明，微量添加晶界合金几乎不影响烧结Nd—Fe—B磁体的磁性能。     

Nd-Fe-B磁体烧结致密化过程的研究

定量描述了Nd-Fe-B磁体的烧结致密化过程, 分析了有效稀土含量、合金粉末粒度与烧结致密化过程的关系, 讨论了Nd-Fe-B磁体烧结过程的致密化机制. Nd-Fe-B磁体烧结致密化过程可分为3个阶段, 即致密化过程迅速进行阶段、缓慢进行阶段、相对稳定阶段;随着烧结温度的上升, 第一阶段表现得更为突出, 第二阶段对应的烧结时间区段大大缩短. 有效稀土含量的提高、合金粉末粒度的减小显著促进Nd-Fe-B磁体烧结致密化过程. 主相颗粒重排以及主相颗粒长大与形状适位性变化是Nd-Fe-B磁体烧结过程的两类主要致密化机制, 而且后者对于Nd-Fe-B烧结磁体实现完全致密化起着决定性的作用.     

烧结过程对Nd-Fe-B永磁材料磁性能与力学性能的影响

分析了烧结过程对Nd-Fe-B永磁材料磁性能和力学性能的影响.当烧结温度为1 373 K时,随烧结保持时间延长,材料剩磁Br先增加后趋于稳定,矫顽力Hci直线下降.成分为Nd25.5Pr7.5FebalNb0.45Cu0.2Al0.55B1.10的磁体样品的抗弯强度在烧结时间为5 h时达到一个最大值后便持续下降,而成分为Nd25.5Pr7.57.5FebalNb0.15Cu0.25Al0.75B1.10的磁体样品抗弯强度是持续下降的.试验结果表明:通过优化合金成分和烧结工艺参数,可以改善烧结Nd-Fe-B永磁材料的磁性能和力学性能,获得综合性能较高的磁体.     

纳米La_2O_3掺杂对Mo_2NiB_2基金属陶瓷组织及力学性能的影响

采用真空热压烧结技术,根据Ni-6B-53.3Mo的配比,制备了掺杂不同含量纳米La_2O_3颗粒(0、0.3%、0.6%、0.9%、1.2%)的Mo_2NiB_2基金属陶瓷,并研究其显微结构和力学性能。结果表明,掺杂La_2O_3可以使Mo_2NiB_2基金属陶瓷的硬质相和Ni基粘结相相溶性提高,晶粒尺寸减小,Ni基粘结相分布更加均匀。随着La_2O_3掺杂含量的增加,Mo_2NiB_2基金属陶瓷的抗弯强度、硬度和压缩强度先增大后减小。掺杂0.6%La_2O_3时,抗弯强度和硬度均最大,分别为603.55 MPa和902.1 HV。掺杂0.3%La_2O_3时,压缩强度最大,为550 MPa。但随着La_2O_3掺杂含量的增加,Mo_2NiB_2基金属陶瓷的断裂韧性和密度都有所降低。     

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.     

晶界扩散Tb对烧结Nd-Fe-B组织与磁性能的影响

用磁控溅射法在烧结Nd-Fe-B磁体表面沉积Tb金属薄膜并进行晶界扩散处理,对比经不同热扩散温度及时间处理后的磁体组织和磁性能变化。结果表明,925℃×10 h+500℃×2 h为最佳晶界扩散工艺,可将磁体矫顽力提高到1630.9 kA·m^-1,较原始磁体提升50%,同时剩磁和磁能积无明显下降,磁体仍具有较高的退磁曲线方形度。晶界扩散处理后磁体取向度有所提高,主相晶粒表面形成了明显的富Tb壳层结构,其厚度随离开磁体表面距离的增加逐渐变薄,随热扩散温度升高和时间延长逐渐增厚。长时间热扩散处理使磁体内形成沿晶界分布的连续薄层富Nd相,将主相晶粒彼此分隔,有效降低磁性相颗粒间交换耦合作用。能谱(EDS)分析表明,适当的热扩散工艺可使Tb元素扩散至磁体芯部,渗透厚度4 mm的磁体。     

注射成形粘结钕铁硼/铁氧体复合磁体的研究

对注射成形粘结Nd-Fe-B/铁氧体复合磁体进行了深入的研究。实验结果表明：随着铁氧体磁粉的加入，复合磁体的磁性能虽略有降低，但其力学性能及热稳定性均有大幅度改善，特别是在铁氧体含量为87%（质量分数时），复合磁体内禀矫顽力温度系数为零，不同磁粉间静磁场的存在，使得复合磁体在铁氧体含量低于70%（质量分数）时，其磁性能大于平均值，而大于70%（质量分数）时则小于平均值。     

稀土含量对烧结NdFeB磁体磁性能及力学性能的影响

研究了不同稀土含量的烧结NdFeB磁体的磁性能、微观结构和抗弯强度。结果表明,提高稀土含量可提高烧结NdFeB磁体的抗弯强度,同时对烧结NdFeB磁体的矫顽力和退磁曲线方形度有一定的提高作用,但会降低烧结NdFeB磁体的剩磁。SEM微观形貌图像表明,提高稀土含量可有效改善铸片、烧结NdFeB磁体的微观结构,使富稀土相分布更加均匀连续,从而提高烧结NdFeB磁体的抗弯强度和矫顽力。     

Influence of dysprosium substitution on magnetic and mechanical properties of high intrinsic coercivity Nd-Fe-B magnets prepared by double-alloy powder mixed method

The double-alloy powder mixed method is very proper for developing new small-mass products by changing the composition of sintered Nd-Fe-B magnets, and there is little research on this aspect. The variation on magnetic and mechanical properties of high intrinsic coercivity Nd-Fe-B magnets prepared by double-alloy powder mixed method was discussed, which is a method blending two-type main phase alloy powders with different components. The results showed that the intrinsic coercivity and density of sintered Nd-Fe-B magnets increased gradually with the increase in Dy content, and the double-alloy powder mixed method could obtain high intrinsic coercivity Nd-Fe-B magnets with good crystallographic alignment and microstructure. The bending strength of sintered Nd-Fe-B magnets declined, and the Rockwell hardness of sintered Nd-Fe-B magnets first declined, and then increased with the increase in Dy content. The microstructure showed that there existed the phenomenon that the Dy element diffused into main phase during sintering process, and the distribution of Dy content in main phase had some variation in homogeneity as a result of incomplete reaction between the double-alloy powder types.     

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.     

Corrosion resistance and mechanical properties of (Ho,Nd)FeB magnets

(Ho,Nd)FeB magnets with different Ho contents were prepared by Ho substitution for part of Nd during the casting process. Effects of Ho contents on the corrosion resistance and mechanical properties of (Ho,Nd)FeB magnets were analyzed by a highly accelerated aging tester, an electrochemical workstation, a microhardness tester, a bending tester, a scanning electron microscope and an X-ray diffractometer. Results show that the addition of Ho can change the main phase structure, optimize the distribution of rare-earth rich (RE-rich) phases in grain boundary, and improve the corrosion resistance and mechanical properties of NdFeB magnets. When the content of Ho increases from 0 to 21.0 wt%, the weight loss of magnets decreases from 2.672 to 0.933 mg/cm², and the microhardness and bending strength increase from 528.74 HV and 374.92 MPa to 633.84 HV and 459.80 MPa, respectively.     

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。     

Effects of Nd–Ga intergranular addition on microstructure and magnetic properties of heavy-rare-earth-free Nd-Fe-B sintered magnets

In this study, we propose an approach of grain boundary modification that can significantly increase the coercivity of the B-lean Nd-Fe-B sintered magnets by intergranular addition of Nd–Ga. The coercivity is substantially enhanced from 1.51 to 2.04 T through optimizing the microstructure and adjusting the phase composition for the grain boundary phase in the annealed magnets. The matrix grains are covered by a continuous thin grain boundary phase accompanying the formation of intermetallic Nd₆Fe₁₃Ga phases. The analysis of magnetic behaviors above Curie temperature confirms that the grain boundary phase of annealed Nd–Ga doped magnets appears to be non-ferromagnetic, facilitating the intergrain exchange decoupling. Microstructure observation in grain boundary area indicates that some surface of the matrix grain is dissolved in the formation process of the Nd₆Fe₁₃Ga phase. It gives rise to a decrease in the proportion of matrix grains and saturation magnetization of the magnet. The detailed relationship between magnetic properties and microstructure is discussed based on these results.     

Preparation and characterization of sodium silicate/epoxy resin composite bonded Nd-Fe-B magnets with high performance

As an organic binder for bonded Nd-Fe-B magnets, epoxy resin(EP) has poor heat resistance but good moisture resistance, while sodium silicate(SS) has poor moisture absorption but better heat resistance and corrosion resistance. In order to improve high temperature stability and decrease moisture absorption of bonded Nd-Fe-B magnets, EP/SS composites were applied as the binder to prepare bonded Nd-Fe-B magnets. The magnetic properties, moisture absorption, corrosion resistance, compressive strength and microstructure of composite bonded magnets were investigated. The results show that EP/SS bonded magnets can obtain excellent magnetic properties at room temperature, and even useable magnetic properties a thigh temperature environments at 200°C. EP/SS composite binder effectively improves heat resistance and corrosion resistance of bonded Nd-Fe-B magnets, and reduces the hygroscopic properties. The molecule of sodium silicateis rigid and keeps it original shape at high temperature environments. In addition, SS in composite binder improves the mobility of the magnetic powders during the pre-pressing process, which makes the magnetic powders attain a more regular structure. These two factors will increase the mechanical properties. Moreover, sodium silicate in the composite binder can also cover the surfaces protecting the magnetic powders from oxidation and corrosion. EP in composite binder can cover SS surface to reduce the water absorption of SS as epoxy is a hydrophobic material. The EDX analysis shows that the composite binder has accumulated in the gaps of the magnet powders, which not only improves heat resistance and corrosion resistance, but also increases the mechanical properties. Therefore, EP/SS composite binder endows bonded Nd-Fe-B magnets excellent comprehensive properties.     

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.     

(Nd,Pr,Ce)-Fe-B磁体的组织与磁学性能

为开发低成本烧结钕铁硼磁体,用30% Ce替代(Nd_0.75Pr_0.25)_32.69Fe_66.25B_1.06磁体中的Nd和Pr,研究了磁体在烧结及回火过程中的组织结构和磁学性能变化.结果表明,取向压坯在1030~1080℃烧结2 h后,随烧结温度升高,磁学性能下降,烧结温度为1030℃时综合磁学性能均最好.烧结态Ce替代磁体的综合磁学性能优于未替代磁体.一级回火后,相组成和晶粒尺寸基本不变,边界结构也未发生明显变化,磁体性能基本不变,或有少量下降.二级回火后,晶界明显改善,获得较清晰且平直的晶界,磁体矫顽力均得到大幅提高.Ce替代磁体的剩磁、矫顽力和磁能积均稍低于未替代磁体.