优化边界结构改善烧结Nd-Fe-B永磁材料的力学性能

在富稀土辅合金中添加Co,Nb,Ti,Ga,Al等元素,用双合金工艺制备一系列不同辅合金含量的烧结Nd-Fe-B磁体,对力学性能进行系统研究。结果表明,在主合金(NdDyTb)12.69(FeCoNb)84.01B6.00的基础上添加3.0wt%的(NdDyTb)25(FeCoNbTiGaAl)68B7富稀土辅合金,其抗弯强度从316MPa提高到344MPa,抗弯强度的改善来自于边界结构的改善以及一些新相的生成。当辅合金含量达到8wt%,合金的强度又下降为321MPa。还研究了热处理工艺对Nd-Fe-B永磁材料力学性能的影响,含3.0wt%辅合金的磁体抗弯强度由烧结态的291MPa提高到最佳回火态的344MPa,又下降为非最佳回火态的304MPa。     

Statistical model of magnetization reversal in Nd-Fe-B sintered magnets

Statistical model of magnetization reversal was used to simulate the magnetization reversal behavior in the sintered Nd-Fe-B magnets with double grain-size distributions due to the abnormal grain growth (AGG). The magnetic properties and mechanical properties due to the formation of AGG grains in Nd-Fe-B sintered magnets were tested. The results show that the magnetic properties, especially the rectangularity were severely deteriorated after the formation of the AGG grains and a step was shown on the demagnetization curve, and the occurrence of AGG mayaccount for the poor rectangularity and existence of the step on demagnetization curve according to the statistical model of magnetization reversal. The fracture toughness and bending strength are lowered because of the stress concentration in the AGG grains. The SEM images show that the formation of AGG grains is caused by the solid sintering due to the absence of RE-rich phase. Statistical model of magnetization reversal can qualitative by explain the dependence of the magnetization reversal behavior on the grain size in the Nd-Fe-B sintered magnets.     

碳对烧结Nd-Fe-B永磁体性能的影响

本文采用两种不同碳含量的原料铁棒,按相同的传统烧结Nd-Fe-B永磁体的工艺,制得NdDyAlCuBFe块状永磁体,研究了碳对烧结Nd-Fe-B永磁体性能的影响.结果显示,原料铁棒中C含量增高,磁体的磁性能如剩磁、矫顽力、磁能积以及方形度都下降.SEM和金相显微观察表明:高C含量中的Nd2Fe14B主相的晶粒大小不均匀,小的为10μm,而大的达到100μm,且富Nd相分布也不均匀;而低C含量中的Nd2Fe14B主相的晶粒细小均匀,约为10～20μm,而且富Nd相分布均匀.造成上述差别的原因是:C是一种杂质元素,呈负电性,易与Nd发生反应,在晶界形成富C、富Nd的第二相杂质,破坏Nd2Fe14B主相,从而使磁体的各项磁性能指标都下降.     

Magnetic properties and thermal stability of anisotropic bonded Nd-Fe-B magnets by warm compaction

Anisotropic bonded magnets were prepared by warm compaction using anisotropic Nd-Fe-B powder. The forming process, magnetic properties, and temperature stability were studied. The results indicate that the optimal temperature of the process, which was decided by the viscosity of the binders, was 110℃. With increasing pressure, the density of the magnets increased. When the pressure was above 700 MPa, the powder particles were destroyed and the magnetic properties decreased. The magnetic properties of the anisotropic bonded magnets were as follows: remanence Br = 0.98 T, intrinsic coercivity iHc=1361 kA/m, and maximum energy product BHmax = 166 kJ/m3. The magnets had excellent thermal stability because of the high coercivity and good squareness of demagnetization curves. The flux density of the magnets was 35% higher than that of isotropic bonded Nd-Fe-B magnets at 120℃ for 1000 h. The flux density of the bonded magnets showed little change with regard to temperature.     

添加Mg_7Zn_3对烧结Nd-Fe-B抗腐蚀性能及磁性能的影响

研究添加Mg7Zn3合金粉对Nd28.0Dy2.2Al0.1Nb0.2B0.96Febal烧结磁体抗腐蚀性能及磁性能影响。磁体在质量分数为3.5%NaCl溶液中的极化曲线测试表明,添加质量分数0.3%Mg7Zn3的合金粉磁体,icorr从3.278μA/cm2降低到1.602μA/cm2,此时icorr最小,具有最好的抗腐蚀性能。适量添加Mg7Zn3合金粉还能提高磁性能。Mg7Zn3合金粉的添加使晶界相电位得到提高和富钕相分布更加均匀,并细化了Nd2Fe14B晶粒,同时提高了磁体抗腐蚀性能和磁性能。     

Effect of bonding process on the properties of isotropic epoxy resin-bonded Nd-Fe-B magnets

Bonded NdFeB magnets were prepared by compression molding. The effect of preparation technology on their magnetic and mechanical properties was studied through the analysis of density, Br Hcj, (BH)max, bending strength, and compressive strength of the bonded magnets. The results showed that the magnetic properties decreased with increasing binder content, whereas the mechanical properties increased. Brand (BH)max increased with rising pressure, whereas Hcj decreased. For a fixed mass fraction of the binder, the optimal pressure was 620 MPa and the best thermosetting temperature was 160℃. These conditions made the bonded magnets have the optimal mechanical properties. Scanning electron microscopy (SEM) analyses of the fracture surfaces indicated that the epoxy resin bonded magnets exhibited brittle behavior.     

Cu/Al复合添加对烧结NdFeB抗腐蚀性及磁性的影响

研究了Cu/Al复合添加对(Pr, Nd)12.8Dy1.0FebalNb0.1B6.0 (at%)烧结磁体抗腐蚀性和磁性的影响。结果表明：添加0.6 at% Al和0.2 at% Cu时磁体的抗腐蚀性最强,磁体在0.001 mol/L HCl溶液中的腐蚀电流密度从46.90 μA·cm-2降低到11.14 μA·cm-2,在湿热环境中腐蚀100 h的质量损失从13.2 mg·cm-2降低到0.4 mg·cm-2。抗腐蚀性的提高源于Cu和Al对富(Pr, Nd)晶界相化学稳定性的提高及其分布状况的改善。同时,Cu/Al对烧结NdFeB晶界结构的优化也有利于磁体磁性能的提高     

Influence of dynamic crystallization on exchange-coupled NdFeB nanocrystalline permanent magnets

Dynamic crystallization was introduced to improve the magnetic properties of NdFeB nanocrystalline permanent magnets by optimizing microstructure. The microstructure was studied by X-ray diffraction (XRD) and transmission electron microscopy (TEM). It has been determined that, compared with the conventional heat treatment, dynamic crystallization can shorten the crystallization time. Moreover, dynamic crystallization can refine grains, enhance the exchange-coupled interaction among grains, and promote the magnetic properties. As a result, the optimal magnetic properties of Nd10.5(FeCoZr)83.4B6.1(Br＝0.685T, Hci ＝732 kA·m -1 , Hcb ＝429 kA·m-1 ,( BH )m=75 kJ·m -3 ) are obtained after dynamic crystallization heat treatment at 700 ℃ for 10 min.     

Research of warm compaction technology on nylon bonded Nd-Fe-B magnets

Warm compaction and room temperature compaction were applied to prepare bonded Nd-Fe-B magnets. The results indicated that the density of magnet was determined by the compaction pressure and warm compaction temperature, whereas, the thermosetting temperature could hardly affect the density of magnet. The mechanical properties of magnets were the best when the thermosetting temperature was 200 ℃. The Br, Hcb, and (BH)max of warm compaction magnet were higher than those of room compaction. When the warm compa...     

热处理对烧结NdFeB磁体微观结构和磁性能的影响

系统研究了热处理对烧结NdFeB磁体微观结构和磁性能的影响.结果表明：二级回火热处理后,磁体微观组织结构得到明显改善,晶界变得更加规整、平滑,富Nd相均匀弥散地分布于晶粒周围,晶界相成分趋于稳定、均匀;磁体的内禀矫顽力显著提高,剩磁及最大磁能积也有一定程度的提高,极大地改善了磁体的热稳定性.     

雾化喷涂沉积对晶界扩散Nd-Fe-B磁性能和微观结构的影响

提出了一种新的雾化喷涂沉积（SCD）方法,在Nd-Fe-B磁体表面均匀沉积TbF₃粉末,同时通过晶界扩散过程（GBDP）将Tb元素引入到磁体中。用这种方法（SCD+GBDP）处理厚度达5 mm的钕铁硼磁体。研究了TbF₃涂层增重比、扩散时间和扩散温度对烧结磁体组织和磁性能的影响。样品扩散温度和时间为940 ℃和10 h,退火温度和时间为480 ℃和5 h。TbF₃增重比（w）从0%增加到0.8%时,磁体的矫顽力从1201 kA/m 提高到1930 kA/m,剩磁下降约0.01 T。研究发现,随着TbF₃增重比的增加,磁体的矫顽力先增大后减小。SEM结果表明,在Nd₂Fe₁₄B晶粒边界区域,Tb取代Nd形成(Nd, Tb)₂Fe₁₄B核壳相。晶界相和核壳相中较高的磁晶各向异性对矫顽力的增强有积极的促进作用。核壳相的分布和浓度对矫顽力有密切的影响。当TbF₃增重比大于2.4%时,靠近磁体表面区域的晶界扩散明显增强。元素的SEM图像显示,进入磁体的Tb越多,晶核内的Tb浓度就越高。此外,大量Nd-F/Nd-O-F相的形成导致晶界相不像w=0.8% 时的样品那样连续,这可能是导致矫顽力下降的主要原因。     

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.     

合金元素对(NdPr)_6Fe_(79)B_(15)非晶厚带的晶化行为及磁性能影响

利用熔体快淬法制备了(Nd Pr)6Fe79B15和(Nd Pr,Dy)6Fe74.5Co3Cu0.5Zr1B15非晶带。通过X射线衍射(XRD)和差热分析(DSC),并借助Kempen模型和Kissinger方程,研究了合金的非晶晶化过程及非等温晶化动力学。结果表明,与(Nd Pr)6Fe79B15合金相比,(Nd Pr,Dy)6Fe74.5Co3Cu0.5Zr1B15合金的非晶形成能力明显提高,在9 m/s的辊速下获得了厚度为100μm以上的非晶厚带。2种合金的非晶厚带具有不同的晶化过程及晶化动力学机制。(Nd Pr)6Fe79B15合金的晶化分4步完成:非晶相(A)→Nd2Fe23B3+A’→α-Fe+Fe3B+Nd2Fe23B3’→α-Fe+Fe3B+Nd2Fe14B→α-Fe+Fe3B+Nd2Fe14B+Nd1Fe4B4;而(Nd Pr,Dy)6Fe74.5Co3-Cu0.5Zr1B15合金的晶化分两步完成:非晶相(A)→Fe3B+A’→α-Fe+Fe3B+Nd2Fe14B。与(Nd Pr)6Fe79B15合金由界面控制的多晶型晶化不同,(Nd Pr,Dy)6Fe74.5Co3Cu0.5Zr1B15合金第1步为界面控制的多晶型晶化,第2步则以扩散控制的共晶型晶化为主。由于退火后组织结构的细化和改善,(Nd Pr,Dy)6Fe74.5Co3Cu0.5Zr1B15合金带的磁性能明显优于(Nd Pr)6Fe79B15合金带。     

Magnetic microstructure and coercivity mechanism of high performance Nd-Fe-B magnets

Magnetic microstructure of high performance Nd-Fe-B magnets was investigated by using magnetic force microscopy. The correlation between magnetic microstructure and coercivity for high performance Nd-Fe-B magnets was studied. It is found that the magnets with different coercivity mechanism take on different microstructures and magnetism. Moreover, the magnetic microstructures of high performance permanent magnets can be explained by the starting field theory model.     

一级回火和烧结温度对掺Dy2O3的Nd-Fe-B磁性能影响

研究了一级回火和烧结温度T对掺Dy2O3烧结钕铁硼磁体的磁性能和微观结构的影响.结果表明:一级回火和烧结温度对磁体磁性能影响显著,尤其对矫顽力Hcj的影响.当添加2%(质量分数,下同)的Dy2O3时,一级回火可以明显提高磁体的Hcj,但烧结温度影响甚微;当添加5%的Dy2O3时,随烧结温度的提高,磁体的Hcj显著提高,但是一级回火使Hcj提高不明显.这主要归因于:一是Dy2O3发生置换反应生成Nd2O3颗粒影响烧结和回火制度,二是烧结温度影响Dy原子扩散.     

烧结NdFeB磁体热压变形后富Nd相的显微组织

采用热压变形法对NdFeB磁体晶间富Nd相的显微组织进行了研究,实验结果表明,NdFeB磁体经真空热压变形后,富Nd相不再平均地分布在磁体晶间,而是聚集成团块状或从磁体边缘渗出,显微组织分析表明,富Nd相主要是由α-Dd和Nd2Fe17两相组成,与Nd-Fe合金的共晶组织成分接近,对于晶间添加Al元素的磁体,Al溶入晶间形成Nd2Fe15Al2相弥散地分布在晶界上,这有益于磁体矫顽力的提高;对于晶间添加Cu元素的磁体,晶间没有发现有新相产生。     

Possible methods of recycling NdFeB-type sintered magnets using the HD/degassing process

With the rapid growth in the use of NdFeB-type magnets and with the growing environmental need to conserve both energy and raw materials, the recycling of these magnets is becoming an ever important issue. In this paper it is demonstrated that hydrogen could play a vital role in this process. Fully dense sintered NdFeB-type magnets have been subjected to the hydrogen decrepitation (HD) process. The resultant powder has been subsequently processed in one of two ways in order to produce permanent magnets. Firstly, the powder was subjected to a vacuum degassing treatment over a range of temperatures up to 1000 °C in order to produce powder that would be suitable for the production of anisotropic bonded or hot pressed magnets. Secondly, the HD-powder has been used to produce fully dense sintered magnets; in which case optimisation of the milling time, sintering temperature and time was carried out. The optimum degassing temperature for coercive powder was found to be 700 °C, giving powder with a remanence (Br) of 1350 mT (±50 mT) and an intrinsic coercivity (Hcj) of 750 kA m⁻¹ (±50 kA m⁻¹). The best sintered magnet was produced by very lightly milling the powder (30 min, roller ball mill), aligning, pressing and vacuum sintering at 1080 °C for 1 h. The magnetic properties of this magnet were: (BH)_max = 290 kJ m⁻³ (±5 kJ m⁻³), Br = 1240 mT (±50 mT) and Hcj = 830 kA m⁻¹ (±50 kA m⁻¹); representing decreases of 15%, 10% and 20%, respectively, from the properties of the initial magnet.     

Nd9.5Fe81Zr3B6.5纳米复相永磁材料的物相演变及磁性能

利用单辊快淬法制备Nd9.5Fe81Zr3B6.5合金条带,采用X射线衍射、差式扫描热分析、透射电子显微分析和振动磁强计等分析测试手段,对合金条带的物相演变和磁性能进行研究。结果表明：在不同快淬速度的条件下,合金条带的微观组织结构不同;在热处理过程中,合金的晶化过程分两步完成：α-Fe 首先析出,Nd2Fe14B 随后析出。随着快淬速度的增大,最佳热处理后合金的晶粒变粗,这使得软磁相和硬磁相之间的交换耦合作用减弱,进而导致合金磁性能的降低。     

磷化温度对烧结Nd-Fe-B永磁合金表面磷酸盐化学转化膜组织结构和耐蚀性能的影响

研究了磷化温度对烧结钕铁硼永磁合金表面磷酸盐化学转化（PCC）膜的形成、微观结构和耐蚀性能以及对磁体磁性能的影响。结果表明,随着磷化温度的升高,转化膜膜重略有增加。扫描电镜观察结果表明,转化膜呈块状结构,晶粒尺寸为5~10 μm。能量色散谱和傅里叶变换红外光谱测试表明,转化膜主要由钕磷酸盐水合物、镨磷酸盐水合物和少量铁磷酸盐水合物组成。转化膜中的氧、磷元素主要分布在晶粒表面,铁元素主要集中在晶界处,钕和镨的分布则比较均匀。电化学分析和静态全浸腐蚀试验表明,不同温度下制备的转化膜均可以提高烧结钕铁硼永磁合金的耐蚀性能。在70 ℃下制备的转化膜由于组织结构均匀致密,具有更好的耐蚀性能。磷化处理后,样品的磁性能均有所下降,但是70 ℃下处理的样品性能相对较好。因此,烧结Nd-Fe-B永磁合金的最佳磷化温度为70 ℃。     

磁粉粒径对烧结Nd-Fe-B磁性能和初始磁导率的影响

采用粉末冶金法制备了名义成分为(Pr_(25)Nd_(75))_(25)Dy_6Al_(0.5)B_1Co_1Cu_(0.2)Fe_(bal)的烧结Nd-Fe-B磁体,并研究了不同粒径磁粉制备的烧结Nd-Fe-B磁体磁性能和初始磁化阶段最大磁导率的相应演变规律。结果表明,磁粉平均尺寸为3.0μm时对应的磁体的内禀矫顽力最大,磁粉平均尺寸为3.5μm时对应的磁体的剩磁最高。从磁体的微观结构观察和性能测试发现,磁粉粒径为3.0μm时,烧结磁体主相更加规则、均匀,提高了磁体的矫顽力。随着磁粉平均尺寸进一步减小,磁粉粒径为2.5μm时,富Nd相以氧化物形式发生了团聚,且分布不均匀,磁体晶界出现孔洞,去磁耦合效率下降,导致磁体矫顽力降低;磁体氧含量随着磁粉平均尺寸的减小而增大,磁体内杂质相增多,剩磁下降;增多的杂质相使得磁化初始阶段的最大磁导率降低。