Sm2Co17型高温稀土永磁的微结构与磁性能

采用透射电子显微镜（TEM）、扫描电子显微镜（SEM）、磁力显微镜（MFM）和原位X射线衍射（XRD）等探讨Sm2Co17型稀土永磁材料的胞状结构、畴结构和相结构及其对磁性能的影响,制备使用温度为500℃的高温稀土永磁材料。结果表明,Sm（CoFe0.11Cu0.10Zr0.03）7.5具有很好的高温稳定性,500℃时的磁性能为：Br=0.708 T,Hci=646.7 kA/m,BHmax=85.4 kJ/m^3;其磁畴宽度远小于晶粒尺寸,但大于胞状结构的尺寸,使用温度较高的磁体具有较小的磁畴和胞状结构;当使用温度小于300℃时,Sm2Co17型磁体内存在的相结构为2：17R、2：17H和1：5相,矫顽力主要受1：5相的钉扎而产生;当300℃〈t〈tc^1：5时,部分1：5相转变成中间相并最终转变成2：7相,磁体的矫顽力将由1：5相钉扎和2：7相形核所控制;当t≥tc^1：5时,磁体的矫顽力将全部由非磁性1：5相和2：7相形核所控制。     

Sm2Co17基高温稀土永磁材料的显微结构与磁性

Cu含量较高的Sm2Co17基永磁材料在高温下具有较大的内禀矫顽力,而Fe含量较高时其高温下的磁性较差．TEM显示磁体由胞状结构构成,胞内为2：17R相,胞壁为1：5相,在MFM（磁力显微镜）下可观测到片状相（1：7相）,畴结构为波纹畴和条状畴,但是在片状相出现的区域并未观察到畴壁钉扎点,而在胞壁相的三角结合区域畴壁的钉扎强度最高,高温X射线衍射分析表明,随着性能的降低观测到材料的相结构发生了较大的变化,由室温下的2：17R主相、1：5相和1：7相变为非晶结构,且最终转变成700℃时的SmCo3主相和2：17R相,相结构的转变直接导致磁体性能的降低。     

Temperature stability and microstructure of ultra-high intrinsic coercivity Nd-Fe-B magnets

The variations of intrinsic coercivity and remanence of sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity were investigated. The results showed that the intrinsic coercivity and remanence declined simultaneously with increasing temperature, but the squareness of the magnets has hardly been changed. The temperature coefficients of remanence （α） and coercivity （β） for the magnets were calculated by two different methods, and the variations of the temperature coefficients and the microstructure of sintered Nd-Fe-B magnets were analyzed. The temperature coefficients of remanence （α） and coercivity （β） for the sintered magnets are very small, and the existence of fine microstructure is necessary to obtain sintered Nd-Fe-B magnets with ultra-high intrinsic coercivity.     

时效处理对Sm2Co17型稀土永磁的磁性能和扩散长度的影响机制

研究一级时效、两级时效和多级时效处理对Sm（CoFe0.20Cu0.12Zr0.03）7.5磁性能的影响,并引入扩散长度探讨材料时效处理动力学机制。结果表明,一级时效处理的温度越高,材料的扩散系数DT1越大,达到某一特定扩散长度所需的时间越少,即磁体达到矫顽力峰值所需的时间越短。在连续降温处理过程中,达到某一特定扩散长度所需的时间与降温幅度和扩散系数有关,Cu原子的扩散长度是连续降温时效处理过程的主要影响因素。Sm2Co17型永磁材料的典型显微结构是由2-17R主相和1-5胞壁相所组成的胞状结构以及片状结构构成。当一级时效温度T1和二级时效温度T2固定时,达到特定扩散长度所须的时间与这2个温度下磁体的扩散系数成反比。Cu原子沿片状相的扩散速率比沿晶内体扩散速率大,当磁体内片状相含量较多时,Cu原子的扩散系数可大大增加,可有效缩短扩散所需时间。     

Investigation of the coercivity mechanism for Nd-Fe-B based magnets prepared by a new technique of strip casting

The coercivity mechanism of Nd-Fe-B based magnets prepared by a new technique of strip casting was investigated. Different from the traditional magnets, α-Fe phases are difficult to be found in Nd-Fe-B magnets prepared by strip casting. Meanwhile, the rich-Nd phases occur not only near the grain boundaries of main phases, but also within the main-phase grains. Investigation on the magnetizing field dependence of the eoercivity for the (Nd0.935Dy0.065）14.5Fe79.4B6.1magnet and the temperature dependence of the coercivity for the Nd14.5Fe79.4B6.1magnet have been done. Results show that coercivities for strip casting magnets are controlled by the nucleation mechanism.     

SC工艺制备Sm2Co17型永磁材料的金相组织与磁性能

采用SC工艺和通用的熔炼工艺制备了Sm2Co17型永磁材料。对两种工艺所制备的合金金相组织、永磁材料的磁性能进行了研究。另外,也研究了合金时效处理对永磁材料磁性能和取向度的影响。结果表明,SC工艺制备的合金获得了希望的柱状晶结构,但其制备的永磁材料磁性能却明显偏低,取向度只有通用熔炼工艺的74%;时效处理能明显提高SC工艺制备的永磁材料的磁性能,且其磁性能与通用熔炼工艺制备的永磁材料相当。     

退火过程对高温Sm2Co17磁体性能的影响

对Sin（Coba1Fe0.07Cu0.088Zr0.025）7.6烧结磁体在不同回火工艺下的室温和高温磁学性质进行了系统研究。结果表明,不同的等温时效温度回火时,磁体剩余磁通密度B,和最大磁能积（BH）max的在室温下不会有太大变化。然而,在高温（500℃）情形下却有很大区别,在790~810℃,获得了最高的（BH）max和矫顽力。所以回火工艺对磁体的高温性能产生了很大影响。通过调整回火工艺,所得到的样品在500℃性能可以达到Hct=5．48kOe,（BH）max12．45MGOe。     

真空退火对镀Al薄膜NdFeB磁体矫顽力和耐蚀性的影响

采用电弧离子镀技术在烧结NdFeB表面沉积一层Al薄膜,并进行真空退火热处理。利用扫描电镜、永磁材料测量系统、电化学工作站和盐雾试验箱等,研究了不同退火工艺对Al/NdFeB试样显微组织、磁性能和耐蚀性的影响。结果表明,随着退火温度的升高,矫顽力先升高后降低,550 ℃退火60 min时矫顽力最高,达到22.41 kOe,较镀态试样增幅7.6%,但耐蚀性有所降低;随着退火时间的增加,矫顽力先降低后升高,550 ℃退火5 min时矫顽力为22.16 kOe,且自腐蚀电流密度较基体NdFeB降低了1~2个数量级。550 ℃退火5 min试样具有较高的矫顽力和较好的耐蚀性能。     

Microstructures and magnetic properties of Ce32.15Co49.36Cu9.84Fe9.65 magnet sintered at different temperatures

The microstructures and magnetic properties of Ce32.15Co49.36Cu9.84Fe9.65 magnet sintered at the temperatures ranging from 1005 to 1105 ℃ were investigated.The results on scanning electron microscopy and X-ray diffraction analysis indicate that the remanence Br of the magnets is mainly influenced by the degree of the easy-axis orientation when sintering temperature is less than 1085 ℃,the rapidly increasing amount of the secondly phase (5∶19 phase) gives rise to the deterioration of the magnetic properties of the magnet above 1085 ℃.Moreover,it is found that intrinsic coercivity Hci is strongly related to the content of copper in the matrix of the sintered magnets.The optimal sintering temperature is located in 1025～1055 ℃,the corresponding magnetic properties of the magnets are Br=0.685 T,Hci=350 kA·m-1,and maximum energy product (BH)m=85.6 kJ.m-3.     

Sm2Co17型永磁合金时效处理的显微结构与内禀矫顽力

采用扫描电子显微镜(SEM)结合X射线能谱仪(EDS)对Sm2Co17型钐钴永磁合金时效处理过程中的显微结构与成分的变化进行分析,揭示该类永磁合金的显微结构在时效过程中随着时效温度和时间的改变而变化的规律,明确正常样品的典型显微结构SEM照片。此方法较光学显微镜的显微结构结果更加准确直观,较透射电子显微镜则有制样简单和分析快速的特点,在产品质量控制中应用效果显著。     

Effects of oxygen and carbon on the magnetic properties and microstructure of Sm2Co17 permanent magnets

The research on the sintered Sm2Co17 permanent magnets prepared by metal injection molding is still at the exploratory stage. Carbon and oxygen are two key factors that influence the magnetic properties. In this article, the effects of oxygen and carbon on the properties and microstructure of the magnets have been studied. The results indicate that oxygen consumes the effective Sm content of the magnets and forms Sm2O3-the non-magnetism phase, which result in the deterioration of the magnetic properties. Besides, the magnetic properties decrease in evidence with increasing carbon content. The main factor that affects the magnetic properties is the deterioration of the microstructure of the magnets. The Sm（Co, Cu）5 phase decreases, whereas the cell size increases with the increase of the carbon content. When the carbon content is above 0.43 wt.%, the Sm（Co, Cu）5 phase is not enough to form a uniform cellular microstructure. Thus the magnetic properties disappear. ZrC is detected in the magnets by XRD when the carbon content is above 0.21 wt.%. ZrC also reduces the properties of the magnets.     

The influence of Co and Ga additions on the corrosion behavior of nanocrystalline NdFeB magnets

Isotropic nanocrystalline Nd₁₄Fe₈₀B₆ and Nd₁₂Dy₂Fe_73.2Co_6.6Ga_0.6B_5.6 magnets with different grain sizes in the range of 60-600 nm have been produced from melt-spun materials by hot pressing at 700 °C and subsequent annealing at 800 °C for 0.5-6 h. The microstructure has been characterized using XRD, SEM, energy dispersive X-ray analysis, and Kerr microscopy. The corrosion behavior of NdFeB magnets has been examined on 0.1 M H₂SO₄ by in situ inductively coupled plasma solution analysis, gravimetric and electrochemical techniques. The corrosion hydrogen absorption/desorption behavior has been investigated by thermal desorption analysis and hot extraction methods. Partial substitution of Fe with Co and Ga leads to an improvement in corrosion resistance and reduces the affinity and binding energy for hydrogen in these materials. Coarsening of the microstructure results in a better corrosion performance of these materials. The corrosion behavior of the magnets in relation to phase composition, phase distribution and grain size is discussed in terms of dissolution, hydrogenation and mechanical degradation.     

Influence of heat treatment on fracture and magnetic properties of radially oriented Sm2Co17 permanent magnets

The quenching, fracture and aging treatment of radially oriented Sm2Co17 ring magnets were investigated. The results indicate that the ring magnets have obvious anisotropy of thermal expansion, which easily leads to the splits of the magnets during quenching. The fracture is brittle cleavage fracture. The difference （Aa） of the expansion coefficient reaches the maximum value at 800-850 ℃. So, various quenching processes at different steps are adopted in order to reduce the splits. When the magnets are aged, 1：5 phase precipitates from the 2：17 matrix phase and forms a cellular microstructure with 2：17 phase. BHmax and JHc reach the maximum value 226 kJ/m^3 and 2 170 kA/m after being aged at 850 ℃ for 4 h and 8 h, respectively. The aging treatment at 850 ℃ has little influence on remanence（Br）, which can always keep a high value （≥1.0 T）. Through appropriate heat treatment, the ring magnets have uniform cellular microstructure and excellent magnetic properties： Br ≥ 1.0T, JHc ≥2 100 kA/m, BHmax ≥ 220 kJ/m^3.     

Analysis of the temperature dependence of the coercive field of Sm2Co17 based magnets

In Sm₂Co₁₇ based magnets the coercive field is determined by the repulsive or attractive interaction of domain walls with the 1:5 cell walls. With increasing temperature the coercivity mechanism changes from repulsive to attractive pinning and above the Curie temperature of the cell walls a nucleation mechanism may be dominant.     

氧含量对烧结钕铁硼磁体Dy晶界扩散的影响研究

本文主要研究了烧结钕铁硼磁体中氧含量变化对Dy晶界扩散后的Dy含量及矫顽力增加量的影响。选取多种高、低氧磁体进行Dy扩散处理后比较发现,低氧磁体的Dy扩散量和矫顽力提高量均明显高于高氧磁体。对9个0wt.%Dy的不同氧含量样品进行扩散再次确认,氧含量减少有利于Dy扩散量、矫顽力的提高。各样品成分梯度结果显示,低氧磁体的Dy扩散量由表及里全面高于高氧磁体,内外浓度梯度也小于后者。电子探针表征结果表明,低氧磁体Dy扩散后晶界处Dy富集条纹更明显、连续,完整包裹各个主相晶粒。这种结构优化也使低氧磁体各向异性场提高幅度大于高氧磁体。磁体中氧含量降低使富钕相在主相周边均匀连续分布,为后续进入磁体内部的Dy元素提供连续的扩散通道,从而使磁体的Dy扩散量和矫顽力提高量进一步提高。     

纳米双相Nd2Fe14B/α-Fe磁体的微结构和交换耦合作用

用熔体快淬法制备了高性能纳米双相耦合Nd2 Fe14 B/α Fe磁体 ,研究了快淬速率对其微结构和交换耦合作用的影响。实验结果表明 ,控制快淬速率在 12m/s时 ,可直接得到显微组织均匀 ,α Fe相粒子细小且均匀分布的纳米双相耦合Nd2 Fe14 B/α Fe磁体。低温退火消除由快速凝固带来的成分不均匀性后 ,强烈的铁磁交换耦合作用导致其最高磁性能为 :iHc=432 .2kA/m ,Jr=1.0 8T ,(BH) max=115kJ/m3 。快淬速率提高 ,非晶相体积分数增加 ,在高温晶化热处理时软硬磁相析出不均匀 ,个别α Fe相粒子奇异长大 ,尺寸达到 10 0nm左右 ,这不利于软硬磁相间的交换耦合作用 ,有损磁性能。     

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。     

Identification of optimal solid solution temperature for Sm2Co17-type permanent magnets with different Fe contents

It is confirmed that the solid solution tempera-ture range to obtain optimal magnetic properties is different for the magnets with different Fe contents,and the...     

合金元素和退火工艺对电磁纯铁矫顽力的影响

为了使电磁纯铁获得更低的矫顽力,通过利用Thermol-Calc软件计算相变温度、系列温度退火、光学显微组织观察分析、直流磁性能检测等手段研究合金元素和退火工艺对电磁纯铁矫顽力的影响。结果表明,添加1.4%Si、1.0%Mn可使电磁纯铁矫顽力数值降低,继续增加Si、Mn的含量磁性恶化,矫顽力增大,添加0.1%P对矫顽力几乎没有影响。电磁纯铁相变温度A₁为880 ℃时,在A₁-10 ℃退火矫顽力最低;无相变温度时,高温(1100~1200 ℃)退火矫顽力最低。含1.4%Si的电磁纯铁1100 ℃退火后H_c数值(16.85 A/m)最低,满足超级电磁纯铁DT4C的矫顽力要求。     

Preparation of isotropic Sm2Fe17Nx magnetic powders and their bonded magnets

The isotropic Sm2Fe17Nx magnetic powders were prepared by Hydrogenation-Disproportion-Desorption-Recombination (HDDR) process. The phase and microstructure evolutionary process of Sm-Fe alloy during the solidification, homogenization, HDDR and nitration processes were investigated by means of XRD, SEM, EDX and AFM. The results show that the homogeneous Sm2Fe17 alloy wassuccessfully obtained and the impurity phases and residual stress were well removed by heated at 1050 ℃ for 24 h. When heated at 800 ℃ for 1h in H2 of 0.1 Mpa, the alloy turns into SmHx and α-Fe with plenty of nanocrystals. After vacuumized at 800 ℃ for 2h the alloy recombines into Sm2Fe17 with a crystal grain size of about 85 nm.The lattice constant of the alloy increases and the expanding of the crystal cell reaches 6.28% after nitrified at 500 ℃ for 5 h. The magnetic property of isotropic bonded Sm2Fe17Nx magnets is Br=0.6704 T, Hcj = 1015 kA·m-1,( BH )max =73.7 kJ·m-3 with a density of 6.04 g·cm-3 .