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.     

高密度块状钐铁氮磁体制备的研究进展

钐铁氮化合物(Sm₂Fe₁₇N₃)因具有比钕铁硼(Nd₂Fe₁₄B)更高的磁晶各向异性场和居里温度值及更少的稀土含量,成为新型稀土永磁材料研究热点。但是,由于钐铁氮在600℃左右会分解导致永磁性能消失,因此常规的高温烧结工艺并不适用于钐铁氮烧结磁体的制备,现只能将其与高分子材料复合用作塑磁材料,这就导致Sm₂Fe₁₇N₃的磁学性能无法得到充分发挥。因此,开发低温成型工艺制备全金属高密度块状磁体是获取高性能钐铁氮磁体的关键。经过30多年的努力,科研人员已开发出多种制备钐铁氮磁体的低温快速成型工艺,并获得最大磁能积达到199 k J/m³的高性能磁体。本研究将从磁体的制备方法出发,总结当前块状钐铁氮磁体的研究现状及面临的问题,尤其针对不同成型方法出现矫顽力下降的现象提出分析,并对其今后的发展做出展望。     

粘结剂含量对粘结NdFeB磁体力学性能和磁性能的影响

粘结剂作为粘结NdFeB磁体制备过程中的重要组成部分,其作用是提高磁粉颗粒的流动性和粘结强度,保证产品的力学性能和磁性能的稳定。采用理论与实验相结合的方法,研究了粘结剂含量对粘结NdFeB磁体力学性能和磁性能的影响。在此基础上,制备了高性能粘结NdFeB磁体。利用扫描电子显微镜（SEM）对磁体的结构和形貌进行了表征。在NIM-200C磁滞回线仪和电子万能试验机（AG-X plus）上分别测定了环形粘结NdFeB磁体（RSM）的磁性能和力学性能。结果表明,当粘结剂含量为3%（质量分数）时,粘结NdFeB磁体密度最高（5.59 g/cm³）,抗压强度最高（159 MPa）,磁性能最佳。     

磁粉粒度分布和抗氧化剂对注射成型NdFeB粘结磁体性能的影响

本文研究了磁粉的粒度分布以及不同抗氧化剂的加入对注射成型NdFeB粘结磁体密度和磁性能的影响。结果表明，磁粉的粒度分布影响熔体的粘度，适当的粒度分布可以提高磁粉的松装密度和磁体的密度，获得高性能的粘结磁体；抗氧化剂的加入，很好地解决了NdFeB粘结磁体在湿热环境下易氧化生锈的问题，大大提高了磁体的抗氧化性能。     

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.     

热变形温度对纳米晶Nd-Fe-B磁体性能的影响

为了研究纳米晶Nd-Fe-B磁体的热变形机理,在不同温度下对快淬粉进行热压热变形处理.通过分析不同温度下热变形过程中应力和磁体应变的变化,以及磁性能和SEM测试,研究了温度对热变形磁体性能和微观结构的影响,分析了热变形过程的热变形机理.结果表明,纳米晶磁体存在最佳的热压温度和热变形温度.当热压温度为550℃,热变形温度...     

Epoxy resin effect on anisotropic Nd-Fe-B rubber-bonded magnets performance

A novel anisotropic Nd-Fe-B flexible bonded magnet with epoxy resin lubricant was prepared by the two-step method to enhance its performance. Temperature characteristics of epoxy resin and its effect on magnetic properties and preparation of anisotropic Nd-Fe-B flexible bonded magnets were investigated and optimized. DOA of aligned flexible bonded magnets with epoxy resin lubricant increases significantly due to epoxy resin lower viscosity and subsequent better powder particles lubrication at a certain aligning temperature. Meanwhile, H_irr decreases sharply due to improved oxidation resistance of epoxy resin fully encapsulating magnetic powder during magnetic alignment process. Utilizing 1 wt% optimized encapsulating epoxy resin and heating unaligned flexible bonded magnets to 80 °C for 30 min during magnetic alignment resulted in the largest Δ(BH)_max and ΔDOA. Δ(BH)_max increased to over 126% along with ΔDOA increase to over 75%, much higher compared with unaligned flexible bonded magnets prepared exclusively by calendering.     

Fe-Nd-B magnets via the hot extrusion of amorphous powders

A rapid solidification melt spinning technique has been developed to produce amorphous powders of Fe-Nd-B alloys modified with hafnium diboride. The amorphous powders are consolidated by the hot extrusion technique into bulk magnets of various cross sections. Consolidated magnets show ultrafine grain structure stabilized by ultrafine submicron hafnium diboride particles. The extruded magnets develop strong texture-induced magnetic anisotropy which leads to attractive energy product values of up to 16MGOe. Significant improvement in coercivity is also achieved due to ultrafine grain structure of the extruded magnets.     

HOT DEFORMATION OF CAST Pr-Fe-B MAGNETS

The hot deformation process of cast Pr_(19)Fe_(74.5)B_5Cu_(1.5) magnets were studied.It isfound that the easy-axes are aligned parallel to the compressive strain direction in vari-ous hot deformation process.During hot deformation,the crushing of Pr_2Fe_(14)B matrixgrains and the relative slip and rotation between the grains take place and the Pr-richmelt is squeezed out of the magnet,leading to a fine,dense and well-aligned microstruc-ture in the fully-deformed magnets.Magnetic properties of B_r=990 mT,_iH_c=880kA/m and(BH)_m=191 kJ/m~3are obtained.The increase of coercivity is attributed tothe fine Pr_2Fe_(14)B grains and the thin Pr-rich phase layer continuously distributed atthe grain boundaries.The increasing remanence is resulted primarily from the develop-ment of the easy-axis alignment as well as from the densification of the Pr_2Fe_(14)B matrix.The easy-axis alignment is developed by the relative slip and rotation of the crushedPr_2Fe_(14)B grains.A full and slow hot deformation is necessary for the good easy-axisalighnment and high magnetic properties.     

铸造Pr—Fe—B磁体的热压变形研究

研究了铸造Pr_(19)Fe_(74.5)B_5Cu_(1.5)磁体的热压变形过程,结果表明,无论经受何种变形方式,磁体易轴[001]总是沿压缩变形方向取向排列,随着热压变形的进行,磁体发生Pr_2Fe_(14)B主相晶粒的碎化和晶粒间相对滑动和转动,以及富Pr液相被挤出,最终形成细小、致密的取向组织,磁性能提高到B_r=990mT,i_H_c=880kA/m和(BH)_m=191kJ/m~3矫顽力的提高归因于主相晶粒碎化和富Pr相在晶间均匀连续分布,剩磁的提高则主要由已碎化晶粒在变形中相对滑动和转动所形成的易轴取向排列以及主相晶粒的致密化贡献,变形充分而缓慢应是获得较强易轴取向和较高磁性能的重要条件。     

纳米复合稀土永磁材料

综述了近年来稀土永磁材料发展的一个热点方向－纳米复合稀土永磁材料，分析了硬磁相与软磁相的交换耦合作用；对当前制备纳米复合稀土永磁材料的方法，如机械合金化、 熔体快淬法、磁控溅射法和HDDR法等进行了简单介绍；阐述了纳复合永磁材料的特点和改善其性能的方法。     

Recent developments of high-performance NEOMAX magnets

For further improvement in achieving extremely high magnetic properties of Nd- Fe- B sintered magnets, extensive investigation has been done to densify the magnet up to the theoretical value, to increase the volume fraction of the Nd ₂Fe₁₄B matrix phase, and to achieve a high degree of alignment. By controlling chemical composition and the amount of constituent phases,improving particle size distribution, and adopting the isostatic pressing method to get better alignment of fine particles, we have succeeded in obtaining a high-performance magnet having residual flux density (B_r) of 1.495 T (14.95 kG), maximum energy product [(BH)_max] of 431 kj/m³ (54.2 MGOe), and intrinsic coercivity (iH_c) of 845 kA/m (10.62 kOe).     

放电等离子烧结-热变形各向异性Nd-Fe-B磁体的微观组织及磁性能

采用放电等离子烧结及后续热变形技术制备各向异性Nd-Fe-B磁体,研究烧结温度对放电等离子烧结Nd-Fe-B磁体微观组织和磁性能的影响。随着烧结温度在650~900°C范围内的升高,烧结态Nd-Fe-B磁体的剩磁、内禀矫顽力及最大磁能积呈现先升后降的趋势。在800°C下烧结所获得磁体的磁性能最佳。随后,对800°C烧结后具有最佳磁性能的磁体采用放电等离子烧结技术进行后续热变形处理。与初始吸氢-歧化-脱氢-再复合粉末和烧结态磁体相比,热变形磁体拥有更显著的各向异性和更好的磁性能。当热变形温度为800°C且压缩比为50%时,热变形磁体中的Nd2Fe14B晶粒呈扁平片状且不发生异常长大;磁体沿热压方向具有最佳的磁性能：Br、Hcj和（BH）max分别为1.16 T、449 k A/m和178 k J/m3。     

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...     

粘结剂和添加剂对注射成型各向异性粘结NdFeB磁体的影响(英文)

研究了在取向磁场下由HDDR磁粉注射成型的各向异性粘结NdFeB磁体,分析了粘结剂和添加剂对各向异性粘结NdFeB磁体的密度、磁性能以及抗压强度的影响.通过磁粉表面改性,磁粉的抗氧化性能以及磁体的磁性能都得到提高.比较了6种粘结剂对磁体性能的影响,从中得到比较理想的粘结剂,并且考察了抗氧剂以及润滑剂加入量对于磁体性能的影响.试验中,混炼温度为205～215 ℃,注射温度为265℃,注射压力为5～6 MPa,保压时间为5 s,模具加热温度为80℃.制得的磁体的性能为:Br=0.72 T,iHc=983 kA/m,(BH)max=75 kJ/m3.     

温压工艺对粘结NdFeB磁体性能的影响

采用温压工艺制备粘结NdFeB磁体,发现温压技术可以有效地提高牯结磁体的密度.改善磁体磁性能.研究表明:温压效果与温压温度的选择和温压压力密切相关.通过对温压机理的分析,发现最佳温压温度由粘结剂的软化点、粘度和固化点三个因素共同决定.而随着温压压力的升高,粘结NdFeB磁体的密度和磁件能增大,并在压力为650 MPa时得到了粘结磁体磁能积的最大值(50.43 kJ/m~3).     

纳米晶复合永磁材料各向异性的研究进展

具有优良磁性能的各向异性R-Fe-B（R：稀土元素）粘结磁体受到广泛的关注,使用各向异性熔体快淬带制备各向异性粘结磁体工艺较为简单。本文介绍了熔体快淬带织构的形成机理和研究进展,着重于微观结构、添加元素以及处理工艺的影响。     

SPS制备各向异性微米晶SmCo_5烧结磁体的研究

采用放电等离子烧结技术制备了各向异性微米晶SmCo_5磁体,研究了磁体的烧结工艺及添加Fe纳米粉对磁体结构和磁性能的影响。研究发现,SmCo_5烧结磁体的最佳烧结温度为830℃,此时磁体的室温磁性能最佳:B_r=8.19 kGs,H_(cj)=10.6 kOe,(BH)_(max)=13 MGOe;而添加Fe纳米粉的烧结磁体,饱和磁化强度升高,但剩磁和矫顽力降低。XRD结果表明,未添加Fe纳米粉的烧结磁体具有单相CaCu_5结构,而添加Fe纳米粉的烧结磁体出现了2∶17相和Fe-Co软磁相。SEM及能谱分析发现,添加的Fe纳米粉扩散进入了1∶5相,形成Sm(Fe,Co)_5和Sm_2(Fe,Co)_(17))。     

烧结钕铁硼基底成分对晶界扩散效果的影响研究

晶界扩散作为一种能明显提升烧结钕铁硼磁体矫顽力同时实现对重稀土高质化利用的方法,日益成为目前稀土永磁学界和产业界的研究热点。本文利用自动化喷涂设备系统研究了晶界扩散烧结磁体批量制备过程中基底成分差异晶界扩散后磁体磁性能的影响,微观结构和EDS元素分析结果表明：晶界扩散后磁体矫顽力增长幅度的差异,同扩散后磁体内晶粒核壳结构形成充分与否、晶界相均匀分布与否和晶界相铁磁性元素含量高低有密切关联,同时利用晶界扩散工艺制备得到的磁体温度系数要优于传统工艺制备得到的相近似牌号的磁体。     

添加Zr元素对纳米复相Nd10．5Fe78．4-xCo5ZrxB6．1粘结永磁体结构和磁性能的影响

采用快淬、热处理及模压成形工艺，制备了成分为Nd10．5Fe78．4-xCo5ZrxB6．1（x=0，1．0，1．5，2．0，2．5）的5种粘结永磁体。采用XRD,DTA，TEM等方法对合金的组织结构和晶化行为进行了研究。结果表明：Zr含量的增加可提高材料的非晶形成能力；当Zr添加到一定量时，形成高熔点的Fe2Zr相，产生细化晶粒的作用；添加Zr元素显著地提高了合金的矫顽力，改善了退磁曲线矩形度，从而提高了最大磁能积。Nd10．5Fe78．4-xCo5ZrxB6．1永磁体在x=2时获得最佳磁性能，Br=0．659T，Hcj=628kA／m，Hcb=419kA／m，（BH）m=73kJ／m^3。