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.     

烧结合金致密化过程及其对性能的影响

配合发动机高质量气门座的研发，对Fe-Cr-Mo-Ni-Co-C粉末烧结合金致密化过程及其对产品性能的影响进行了实验研究。发现该合金的烧结样密度随生坯密度的提高而提高，当生坯密度较低时，其提高的幅度比较小，当心坯密度在6.5-6.7g/cm^3时，其提高的速度迅速增加，当生坯密度超过6.7g/cm^3，其提高速度减小；还发现该合金烧结密度的变化不仅影响试样孔隙数量的变化，而且影响孔隙形状的变化，因此该合金力学性能随密度的变化曲线并不是一条直线，而是一条分为不同阶段的曲线。还通过该合金的烧结密度对其物理性能的影响，导出了所研究合金于不同湿度时的热导率计算方程，进一步研究该合金的物理性能提供了理论依据。     

压坯密度对烧结NdFeB磁体磁性能的影响

采用速凝片（SC）、氢破（HD）和气流磨（JM）工艺制备钕铁硼磁粉,研究了压坯密度、烧结温度对磁体取向度、微观结构和磁性能的影响。结果表明：选择合理的压坯密度（ρx=3．4g／cm3）可以使磁体在模压和液相烧结过程中保持较高的取向度,剩磁提高约2％。在低温度（1055℃）烧结时,可以获得较为理想的显微组织,主相晶粒细小...     

升温速率对放电等离子烧结铁粉致密化的影响

选用球型雾化铁粉为典型材料,在温度1 075℃、压力40 MPa、保温时间5 min和脉冲8:2的条件下,以不同升温速率(10,30,50,70和90 K/min)进行放电等离子烧结,对烧结体的致密度、微观组织以及致密化动力学等进行分析,研究升温速率对SPS铁粉致密化的影响。结果表明:粉末的SPS致密化过程与传统热压类似,烧结初期致密化速率较大;然后随温度升高,致密化速率加快;烧结后期致密度大幅提高,但由扩散蠕变控制的致密化过程受到晶粒长大的影响,最终致密度趋于稳定。由于保温时间较短,材料的致密度随升温速率提高而减小。提高升温速率能有效抑制样品与模具接触而发生的渗碳行为。     

废旧烧结Nd-Fe-B磁体添加Ce再制造技术研究

烧结Nd-Fe-B磁体再生过程中会引起稀土元素的氧化和损失,因此重新烧结时无法致密化。添加Ce金属,有助于再生磁体的致密化,并优化磁体的显微组织结构。通过低成本Ce金属的添加,成功实现再生磁体的综合性能优化。并研究了废旧烧结Nd-Fe-B磁体的吸氢过程,用BH测试仪测试了再生磁体的磁性能;采用扫描电镜观察了再生磁体的微观结构。添加4%Ce(质量分数)时,在1 350 K烧结、773 K热处理条件下,再生磁体的剩磁达到了原磁体的98%以上,内禀矫顽力超过了原磁体。     

金属注射成形制造音圈马达磁体

全世界每年生产个人电脑硬盘驱动器 2 5亿个以上 ,到 2 0 0 4年销售额将超过 5 0 0亿美元。音圈马达磁体是电脑硬盘驱动器的重要部件 ,通常是由粉末压制—烧结—机加工制成的。这种方法费力、费材且耗能。新的金属注射成形方法是一种经济、简单、不浪费材料、有利环保、可大批量生产的方法。新制造技术介于各向异性注射成形粘结磁体与各向同性压制烧结磁体两种方法之间。首先在磁场中定向压制生坯件 ,而后脱粘结剂 ,最后烧结成全致密的终形件。采用金属注射成形 (ＭＩＭ )技术 ,硬盘驱动器音圈马达磁体的成本可大大降低 ,因为ＭＩＭ具有终…     

工业生产高综合性能烧结 Nd-Fe-B永磁关键技术研究

通过优化合金成分设计和改进合金铸锭按需分配技术、磁场取向成型技术以及烧结技术，应用全部国产设备与国内通用的工业生产烧结Nd-Fe-B永磁的原材料，避免使用镓等稀有贵重金属元素，实现了N45H烧结Nd-Fe-B磁体的工业化生产，其典型磁性能为Br=1.386T(13.86kGs),BHc=1059kA/m(13.32kOe),JHc=1418kA/m(17.83kOe),Hk=1357kA/m(17.06kOe),(BH)max=364kJ/m^3(45.8MGOe)。，SEM观察和XRD分析结果表明，制造的N45H烧结Nd-Fe-B磁体具有良好的取向度和晶粒细小而均匀的显微组织。     

Ce取代量对Nd-Fe-B制备工艺及性能的影响

本文研究了不同Ce添加量对烧结Nd Fe B磁体的制备工艺及磁性能的影响,采用阿基米德法对磁体密度进行测量、脉冲磁滞回线测量仪PFM等对磁体性能进行了分析。研究表明,随着Ce的添加量增加,烧结磁体的密度升高,有利于磁体的致密化。含Ce磁体最佳烧结温区960℃~1010℃之间,比传统Nd Fe B烧结温度低50℃~80℃。随着Ce取代量增加,磁体综合性能下降,Ce含量在30%TRE以上时,热处理对性能的提升效用减弱,磁体只需一步烧结即可达到最优性能,从而缩短了制造流程,为低成本稀土磁体的制备提供了基础。     

细磷铁粉的制备及其对铁粉温压行为的影响

研究了细磷铁粉的制备工艺，并进行了加入细磷铁粉的国产铁粉的温压实验，发现腐蚀球磨法可以有效的细化磷铁份，球磨３６ｈ后的粒度可达１１μｍ，加入细磷铁粉的武钢铁粉可用于无粘结剂的温压工艺提高生坯密度。加入细磷铁粉比粗磷铁粉可能有效地促进烧结致密化过程，孔隙更加细小圆滑。     

微波烧结锇的工艺研究及动力学分析

采用微波烧结技术制备锇（Os）烧结体,研究了生坯压制压强和微波烧结主要工艺参数（升温速率、烧结温度和保温时间）对Os烧结体组织结构和相对密度的影响规律,分析了微波烧结致密化的机理。结果表明,1350 ℃微波烧结后Os平均晶粒尺寸约0.22 μm,与粉体颗粒尺寸差别不大;随着烧结温度增加到1500 ℃,晶粒尺寸长大到0.76 μm。1500 ℃烧结时,延长保温时间,Os烧结体的相对密度先快速增加,后缓慢增加。1500 ℃微波烧结60 min后,Os烧结体相对密度为94.3%,平均粒径小于1 μm。烧结动力学分析表明,Os的致密化过程是体积扩散和晶界扩散共同作用的结果,随着烧结温度的升高,扩散机制从晶界扩散逐渐向体积扩散转变。     

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.     

高性能烧结Nd-Fe-B磁体关键制造技术的开发与应用

烧结Nd-Fe-B永磁材料由于具有低成本、高磁性能而广受人们关注。近20年来，为了提高磁体的磁性能、温度稳定性能和抗腐蚀性能，国内外开展了大量的研究工作。据此，简要综述了近年来高性能烧结Nd-Fe-B磁体关键制造技术的开发与应用状况。     

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.     

Application of Magnetic Field in Fabrication Process of Anisotropic Bonded Nd-Fe-B Magnet

This work studied the application of the different magnetic field used in the compaction process for die fabrication of anisotropic Nd-Fe-B bonded magnet. The static field made from Nd-Fe-B permanent magnets was used in the blending process to separate the particles each other. The SEM observation gave intuitionistic results about it. The anisotropic Nd-Fe-B bonded magnets were fabricated with warm-compaction under the electromagnetic field about 2.5 T. It is known that magnetic field is necessary for anisotropic materials fabrication for alignment. And warm compaction was used to decrease the viscousness of binder, to enhance alignment magnetic particle while press, and to get high density materials. For coercivity of Nd-Fe-B magnets decrease largely with the temperature increasing, press in proper temperature and oriented field is benefit to the magnetic characteristics and the mechanical properties of the anisotropic bonded Nd-Fe-B magnets. Finally solidifying process was performed under the pulse field of 4 T. The increment for solidifying in the field was about 15% for maximum energy product of the bonded magnet. The magnetic properties of anisotropic bonded Nd-Fe-B magnets from d-HDDR powders compact at 90 °C in alignment field of 2.5 T were: B_r=8.55 kGs, _iH_c=12.0 kOe, (BH)_max=14.57 MGOe.     

加剂方式对烧结钕铁硼磁体磁性能的影响

钕铁硼永磁材料在民用、航空航天等众多领域得到广泛的应用。高档次烧结钕铁硼磁体具有良好的市场前景。商业磁体多是由大块烧结毛坯切割而成,磁性能一致性是市场的基本要求之一,润滑剂等化学试剂和磁粉混合不均匀是影响一致性的一个重要因素。钕铁硼磁粉化学性质活泼、容易氧化,制粉的全过程都在氮气气氛下进行,没有合适的设备,想均匀加入化学试剂困难很大。研究人员因设备条件不足无法开展进一步探索。针对这个问题,项目组自行开发了专利产品"自动雾化加剂设备"。通过改变化学试剂加入方式,改善了磁粉和化学试剂混合均匀性,提高了磁体取向度,生产过程中也更好地保护了磁粉,得到内部一致性更好、磁性能更高的烧结钕铁硼磁体:剩磁(Br)=1.426 T,内禀矫顽力(Hcj)=1373.1 kA·m^-1,最大磁能积((BH)max)=406.99 kJ·m^-3。毛坯内部磁性能一致性的提高对后期加工成小片的商业磁体很有意义。开发的"自动雾化加剂设备"已经在烧结钕铁硼行业中得到广泛应用。     

(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.      

Electrochemical Corrosion Behavior of Nd-Fe-B Sintered Magnets in Different Acid Solutions

Electrochemical corrosion behavior of Nd-Fe-B sintered magnets in nitric acid, hydrochloric acid, sulfuric acid, phosphate acid and in oxalic acid was studied. Potentiodynamic polarization curves and immersion time dependence of corrosion rates of Nd-Fe-B sintered magnets in different acid solutions were tested. Microstructures of corroded Nd-Fe-B sintered magnets were investigated by means of SEM and AFM. The results indicate that in strong acid solutions of similar hydrogen ion concentration, the corrosion current increases in the order of HCl 〉 H3SO4 〉 HNO3 solution and Nd-Fe-B sintered magnets are passivated in phosphate acid and oxalic acid. Within 25 min, the corrosion rates of Nd-Fe-B sintered magnets in H2SO4 and H3PO4 solutions show a declining trend with immersion time, while in HNO3 and HCl solutions the corrosion rates are rising. And in H2C2O4 solution, weight of the magnets increases. The brim of Nd-Fe-B sintered magnets is corroded rather seriously and the size of the magnets changed greatly in nitric acid. The surfaces of the corroded magnets in the above mentioned acid solutions are all coarse.     

Improvement of coercivity and corrosion resistance of Nd-Fe-B sintered magnets by doping aluminium nano-particles

Nd-Fe-B permanent magnets with a small amount of Al nano-particles doping were prepared by conventional sintered method. Effect of Al content on magnetic property, corrosion resistance and oxidation properties of the magnets were studied. Investigation showed that the coercivity rose gradually, while the remanence decreased simultaneously with increase of Al doping amount. Further investigation revealed that most Al element diffused into the main phase and some Al element diffused into the Nd-rich phase. The autoclave test results showed that the corrosion rate of the magnets decreased with Al content increasing. After oxidation, the maximum energy product losses of the magnets with 0.0 wt.% and 0.2 wt.% Al nano-particles doping were 6.13% and 3.99%, respectively. Therefore, Al nano-particles doping was a promising way to enhance the coercivity and corrosion resistance of sintered Nd-Fe-B magnet.     

Effect of niobium on thermal stability and impact toughness of Nd-Fe-B magnets with ultra-high intrinsic coercivity

The effects of Nb on the thermal stability and impact toughness of ultra-high intrinsic coercivity of Nd-Fe-B magnets were investigated.The results showed that the addition of Nb could improve the thermal stability,and obviously increased the impact toughness of sintered Nd-Fe-B magnets.The optimum thermal stability of sintered Nd-Fe-B magnets was obtained when the content of Nb was 1.0 at.%.The maximum impact toughness of sintered Nd-Fe-B magnets was obtained when the content of Nb was 1.5 at.%,but the magnetic properties of sintered Nd-Fe-B magnets drastically deteriorated when the content of Nb increased from 1.0 at.% to 1.5 at.%.The microstructure showed that overfull Nb addition made many ultra-fine grains get together,which led to the density of sintered Nd-Fe-B magnets decline and drastically deteriorated the magnetic properties of sintered Nd-Fe-B magnets.