元素Ga对烧结Nd-Fe-B永磁体显微结构与磁性能的影响

本文研究了添加元素Ga[0 %～ 2 % (质量分数 ) ]对烧结Nd15Fe78B7永磁体显微结构与磁性能的影响。结果表明 :添加少量的Ga就可有效的提高内禀矫顽力Hci 而不引起剩磁Br 和最大磁能积 (BH) max 的降低 ;Ga的添加量为 1 0 % (质量分数 )时 ,得到与Nd Fe B系永磁体理想显微结构相近的显微组织结构 ;添加元素Ga在磁体中以Nd2 Fe14 xGaxB和GaNd第二相的形式存在 ;当Ga元素添加量较大时 [>1 5 % (质量分数 ) ]时 ,添加的Ga使主相Nd2 Fe14 B不稳定     

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。     

Ga对(Nd,Dy)—(Fe,Co,Nb)—B稀土永磁体磁性能和显微组织的影响

Ga加入到(Nd,Dy)—(Fe,Co,Nb)—B磁体中,可显著提高其内禀矫顽力iHc,每个Ga原子加入可提高约为147kAm~(-1)。显微组织分析表明,Ga主要分布于富Nd相中,约为硬磁相中Ga含量的10～20倍。Ga主要是通过改变富Nd相的特性来影响矫顽力的。     

Al对(Nd,Dy)-(Fe,Co)-B稀土永磁体磁性能和显微组织的影响

Al可显著提高(Nd,Dy)-(Fe,Co)-B稀土永磁体的矫顽力,降低不可逆损失,δirr<5%的最高温度可达230C。显微组织分析表明,Al对显微组织的影响主要发生在富Nd相内。烧结时,富Nd液相内溶有一定量的Al。冷却时,Al在富Nd相内形成富Al区和含Al量较高的粒子。富Nd液相内的Al可改善其与φ相的湿润性,从而提高磁体的矫顽力。     

添加Gd、Ho对烧结Nd-Fe-B磁体微结构与性能的影响

在Nd-Fe-B合金中添加Gd、Ho元素,可促进Nd2Fe14B柱状晶的生长,使富Nd相分布均匀,细化磁体的晶粒。添加Ho对磁体内禀矫顽力提高较好,添加Gd对磁体J-H退磁曲线的方形度提高较好,但磁体的剩磁与磁能积会降低。Gd、Ho的添加可以降低磁体的开路磁通不可逆损失,使得磁体具有较好的热稳定性。     

液相扩散对钕铁硼磁体性能和组织结构的影响

用双合金工艺在Nd13.05Dy0.23Fe80.12B6.5铸片主合金中分别添加质量分数为3％～20％的富稀土铸锭辅合金Nd38.2Cc11.8Fe44.88Al4.12B,研究在钕铁硼永磁体中用Ce部分地取代Nd时对永磁体的磁性能的变化规律.实验结果表明,在一定的烧结及热处理工艺条件下,辅合金加入量介于8％ ～ 12％(质量分数)时,磁体的内禀矫顽力和磁能积相对较高,对剩磁的影响不大.显微成分分析表明,采用双合金法,使组织中细小的颗粒状富稀土相增多,形成了更多的对矫顽力有贡献的富稀土相,并且富稀土相分布于晶界上.     

磁控溅射法渗镝对烧结钕铁硼性能及显微结构的影响

采用磁控溅射法在钕铁硼表面沉积一层金属Dy,高温扩散后,Dy扩散进入磁体内部,与磁体中Nd发生置换,形成均匀连续的富Nd相,并在主相晶粒表层区域形成(Nd,Dy)2Fe14B相,扩散深度约为350μm。其中,厚度为10 mm的无Dy磁体和低Dy含量磁体添加1%Dy(质量分数)后,经扩散处理,矫顽力分别提高了52.1%和32.2%。结果表明,经磁控溅射法渗镝,钕铁硼矫顽力显著提高,剩磁无明显降低。     

NdFeB磁体耐盐雾腐蚀行为研究

通过中性盐雾(NSS)腐蚀试验,对比分析了烧结Nd Fe B磁体和热变形Nd Fe B磁体在NSS腐蚀环境中的耐蚀行为。研究结果表明,Nd Fe B永磁体的盐雾腐蚀进程可分为两个阶段:腐蚀增重期和失重期,并给出了相应的腐蚀反应速率方程。在NSS腐蚀环境中,热变形Nd Fe B磁体表现出更好的耐蚀性,其失重比高矫顽力烧结磁体降低了30%,认为热变形Nd Fe B磁体具有特殊的片状纳米晶组织结构,富Nd相的晶粒更加细小,分布更加均匀,使得发生晶间腐蚀的通道更窄,从而抑制了腐蚀速率,提高了磁体基体的耐蚀性。     

B 含量对高能积磁体磁性能和耐蚀性的影响

通过调整钕铁硼主元B元素含量研究其对高能积磁体磁性能和耐蚀性的影响,结果表明:磁体中B含量小于5.7%时,合金中出现了易基面的Nd2Fe17相,使Br、iHc都比较低;当添加B超过5.9%时,过量的B形成非磁性的富B相,导致磁体Br下降;当B含量在5.7%～5.9%之间时,磁体有较好的磁性能.显微组织研究表明,B元素影响晶粒的尺寸和形状;磁体耐蚀性能研究表明,当B含量过少或过多时均不利于耐蚀性的提高,B含量在5.76%时为最佳添加量.     

NdFeB-CeFeB互扩散对其组织和磁性能的影响

近年来由于Ce元素的价格优势和特殊性能,Ce掺杂NdFeB永磁体受到越来越广泛的关注。通过900℃均匀化处理、真空扩散焊接和900℃扩散处理制备了NdFeB-CeFeB扩散偶,探究了NdFeB和CeFeB互扩散对各自微观结构和磁性能的影响。扫描电子显微镜(SEM)和能谱分析(EDS)结果发现,随着900℃保温处理时间增长,组织中的第二相和孔洞逐渐消失。互扩散后Ce原子不能置换Nd2Fe14B中的Nd原子,而是主要被富Nd相捕获。而Nd原子扩散后置换Ce2Fe14B中的Ce原子,形成了(Nd0.615Ce0.385)2Fe14B和(Nd0.165Ce0.835)2Fe14B两相,证明(Nd1-xCex)2Fe14B化合物存在溶解间隙。两相区(Ce,Nd)FeB样品中Ce平均原子数约占总稀土原子数的69%,饱和磁化强度μ0MS约为1.46T,各向异性场μ0HA约为7.37T,其磁性能未因高Ce含量而大幅下降主要归功于两相组织的"核壳"结构和Nd对Ce价态的影响。     

纳米复合磁体的开发动向

本文从纳米复合磁体的概念入手 ,综合评述了近年纳米复合磁体的研究结果和开发动向 ,重点介绍了Fe3B/Nd2 Fe14 B系复合磁粉SPRAX的制备工艺 ,纳米晶结构和性能特征。     

Nd2Fe14B/Fe3B基纳米复合粘结磁体的磁特性

通过实验研究了Nd2Fe14B／Fe3B双相纳米复合磁粉分别与几种不同性能的磁粉复合成粘结磁体后磁性能的变化。通过对复合磁体的理论分析得知，由Nd2Fe14B／Fe3B与RE2Fe14B或铁氧体磁粉复合成的粘结磁体中，成分间并未发生化学反应。以Nd2Fe14B／Fe3B铁氧体复合粘结磁体为例，根据理论分析推出的剩磁Br-成分含量关系曲线与实际曲线吻合得很好，表明剩磁与成分含量间存在着近似的线性关系，从而可通过数学手段建立磁性能参数与成分含量的函数关系式，用于简化混粉工艺。另外，添加铁氧体可对该复合磁体较差的热稳定性起到补偿作用，并减少了磁不可逆损失。     

Enhanced magnetic properties in chemically inhomogeneous Nd-Dy-Fe-B sintered magnets by multi-main-phase process

Homogeneous substitution of Dy for Nd in the hard magnetic 2:14:1 phase can effectively enhance coercivity to ensure the high temperature operation,however,inevitably deteriorate remanence at expense.In this work,we performed a comparative investigation of the two magnets prepared by multimain-phase(co-sintering Nd_2 Fe_(14)B and(Nd,Dy)_2 Fe_(14)B powders) and single-main-phase(sintering(Nd,Dy)_2 Fe_(14)B powders) approaches.The comparative investigation reveals that at the same Dy substitution level(2.16 wt%),such chemically inhomogeneous multi-main-phase magnet possesses better roomtemperature magnetic properties as well as thermal stability than those of the single-main-phase one with homogenous Dy distribution in the matrix grains.Room-temperature magnetic properties H_(Cj)=1664 kA/m,B_r=1.33 T and(BH)_(max)=350.4 kJ/m~3 for the multi-main-phase magnet are all better than those for the single-main-phase magnet with H_(Cj)=1536 kA/m,B_r=1.29 T and(BH)_(max)=318.4 kj/m3.In addition,over the temperature range from 295 to 423 K,both the temperature coefficients of coercivity and remanence for the multi-main-phase magnet are also lower than that for the single-main-phase magnet.Such superior magnetic performance is attributed to the short-range magnetic interactions inside individual 2:14:1 phase grains and the long-range magnetostatic interactions between adjacent grains with inhomogeneous Dy distribution.Our work provides a feasible approach of enhancing coercivity and retaining energy product simultaneously in the Nd-Dy-Fe-B permanent magnets.     

Magnetic Properties of Ga Doped Nd-Fe-B Sintered Magnets

The magnetic properties of Nd_(16)Fe_(77)B_7 and Nd_(16)Fe_((61-x))Co_(16)Ga_xB_7(x=0,1,2,4,7)have been measured.Itis found that the remanent magnetization(Br),maximum energy product(BH)_(max)and the Curie temperature(T_c)decrease with the increase of Ga content.The coercive force(He)increases with the increase of Ga contentwhen x is less than 2,but decreases when x>2.At x=2,the coercive force reaches its maximum value.It is alsofound in all the samples investigated that there is a linear relationship between H_c~(1/2)and T~(2/3),which can not beexplained by Gaunt's wall barrier model.The temperature dependence of the calculated values of H_v and(4bf)has been discussed.     

Dependence of magnetic properties on microstructure and composition of Ce-Fe-B sintered magnets

In this paper,dependence of magnetic properties on microstructure and composition of Ce-Fe-B sintered magnets with Cu-doped Ce-rich alloy addition was investigated.It shows that the maximum energy product(BH)_(max) and coercivity H_(cj) of Ce-Fe-B sintered magnet are improved from 6.76 to 9.13 MGOe by 35.1%,and from 1.44 to 1.67 kOe by 16.0%,respectively,via adding 5 wt% liquid phase alloy of Ce_(35.58)Fe_(57.47)Cu_6 B_(0.95)(at%).Compared with the magnet without Cerich alloy addition,the volume fraction of the grain-boundary phase with low melting point increases in the magnet with Ce-rich alloy additio n,which is be ne ficial to imp roving the microstructure and promoting the coercivity enhancement of the magnet.In the Ce-Fe-B magnet with Ce-rich alloy addition,Cu and Ce enrich in the grain boundaries of the magnet after annealing,therefore the as-annealed magnet has a higher coercivity than the as-sintered magnet.A distinct Fe-rich layer with the average thickness of 60 nm is found in the grain boundaries in the magnet without Ce-rich alloy addition,but it seems that Fe-rich phase disappears in the magnet with Ce-rich alloy addition.The present work suggests that the further improvement of coercivity in the Ce-Fe-B sintered magnets is expectable by designing the composition and structure of added liquid phase alloys.     

Effect of Nd3+ substitution on structural and magnetic properties of Mg–Cd ferrites synthesized by microwave sintering technique

Nd~(3+) substituted spinel ferrites with formula Mg_xCd_(1-x)Nd_(0.03)Fe_(1.97)O_4(x = 0.0.2,0.4,0.6.0.8 and 1.0)were prepared by oxalate co-precipitation method using novel microwave sintering technique. AR grade sulphates were used as starting chemicals. The samples were sintered at optimized power of 70 W for10 min in a microwave oven(800 W). The structural analysis of these samples was done by using X-ray diffraction, scanning electron microscope and Fourier transform IR techniques. The XRD analysis of the synthesized ferrite confirms the formation of cubic spinel structure of ferrite. The influence of Nd3+substitution on various structural parameters of Mg-Cd ferrites was reported. IR study indicates the spectra contain two intense absorption bands around 600 and 400 cm~(-1) in addition with four extra bands. The magnetic properties of all ferrites were studied by using a vibration sample magnetometer.The crystallite and grain size dependant magnetic properties are observed. The composition Mg_(0.6)Cd_(0.4)Nd_(0.03)Fe_(1.97)O_4 has better magnetic properties that can be used in recording media. The fast synthesis of spinel ferrites is yielded due to use of the microwave sintering technique.     

Preferred Orientation in Nanocomposite Permanent Magnet Materials

Melt-spun （Nd11.4Fe82.9B5.7）0.99M1 ribbons （M = Zr, Nb, Ga, Zr＋ Ga, Nb ＋ Ga）were prepared by melt-spinning technique. Ga addition is found to be effective for the orientation of c-axis of Nd2Fe14B grains perpendicular to the ribbon plane. Better magnetic properties can be achieved by adding both the two kinds of elements Zr ＋ Ga, Nb ＋ Ga, and it is found that the preferred orientation is further improved. The alignment degree changes with ribbon thickness and is highest when ribbon thickness is 120 μm. Heat treatment can improve the texture degree, but lead to coarser grains. Cryogenic treatment is first applied for the treatment of nanocomposite Nd2Fe14B/α-Fe melt-spun ribbons. The effects on magnetic properties and texture degree of nanocomposite magnets after cryogenic treatment were studied. The result shows that cryogenic treatment is beneficial to the enhancement of texture degree of melt-spun ribbon and the grain size has no obvious change.     

Coercivity enhancement of Ce-Fe-B sintered magnets by low-melting point intergranular additive

Ce-Fe-B sintered magnets with enhanced coercivity were prepared by the powder metallurgy method. The mechanism of the coercivity enhancement in Ce-Fe-B sintered magnets with the low-melting point intergranular additive was discussed in details. It was speculated that the low coercivity of Ce-Fe-B sintered magnet was related to the irregular sharps and relatively low magneto-anisotropy field of the matrix phase. After introducing a 20 wt.% Nd-based intergranular additive, the coercivity markedly increased from 108 Oe to 2560 Oe due to the formation of thin and continuous grain boundary layers and the surface modification of the matrix phase grains. Additionally, the formation of the high anisotropy field(Nd,Ce)_2Fe_(14)B shell was beneficial to the increase of the coercivity as well. This work suggested that adding low-melting point intergranular additives was effective to fabricate the practical Ce-Fe-B sintered magnets.     

Structure and intrinsic magnetic properties of MM_2Fe_(14)B(MM=La,Ce, Pr,Nd) alloys

MM_(33)Fe_(66)B(MM=La, Ce, Pr, Nd) alloys(mass ratio) were prepared by induction melting and heat-treated at 1353 K for 24 h to produce homogeneous MM_2Fe_(14) B phase. The phase structure and element distribution of the alloys were analyzed by X-ray diffraction(XRD) and scanning electron microscope(SEM). The alloys were applied ball milling to obtain powders with good size distribution and then magnetic aligned in a static magnetic field of 2 T for 4 h, in order to achieve the intrinsic magnetic properties by vibrating sample magnetometer(VSM). XRD results showed that the alloys were composed of the single 2:14:1 main phase and RE-rich phase, which was similar to Nd_2Fe_(14)B structure. Magnetic measurements showed that the saturation magnetization(Ms) and anisotropy field(HA) of the MM_(33)Fe_(66)B alloy were 11.3 k Gs and 48.4 k Oe, respectively, demonstrating its good potential as permanent magnets. The Curie temperature of the MM_(33)Fe_(66)B alloy was determined as 502.9 K by magnetization-temperature curves. Microstructure observation showed that Nd and Pr were mainly in the 2:14:1 ferromagnetic phase, while La and Ce prefered to aggregate in the RE-rich grain boundary phase, which is beneficial to fabricating(Pr, Nd, MM)_2Fe_(14)B magnets with good magnetic properties.     

新型(Fe,Co)-Zr-RE-B非晶合金的热稳定性和磁性

利用旋铸技术制备了一种新型的含稀土元素的铁基非晶合金。研究了Nd含量对Fe70Co8Zr7-xNdxB15(x=0～6%原子数分数)合金的非晶形成能力、热稳定性和磁性能的影响。当该合金系的Nd含量在0～6%(原子数分数)变化时,其饱和磁感应强度(Js)在1.10T～1.37T范围内变化,矫顽力(Hc)在2.28A/m～8.15A/m范围内变化。Js随Nd含量的增加而增加,当Nd含量为2%和3%时,其Hc值均在3A/m以下,且在Nd含量为2%时,具有最高的非晶形成能力(glassformationability简称GFA)即大的ΔTx(达61K);同时又有良好的软磁性能,其Js和Hc值分别为1.25T和2.28A/m。经对比得出,Fe70Co8Zr5RE2B15(RE=Ce、Pr、Gd和Tb)合金与Fe70Co8Zr5Nd2B15具有相近的非晶形成能力和磁性能。