烧结钕铁硼磁体晶界扩散Dy/DyFe工艺研究

研究了晶界扩散工艺在烧结钕铁硼中的应用,采用晶界扩散渗Dy/Dy Fe合金的方法,将重稀土元素Dy扩散到烧结钕铁硼磁体内部。在高真空6×10-3Pa下,900℃×3.5 h进行扩散,再在2×102Pa,530℃×3 h下进行回火。选择性地进行追加热处理。研究了此种工艺对烧结磁体的磁性能、磁通不可逆损失和微观组织的影响。结果表明对磁钢进行晶界扩散Dy,使矫顽力增幅为15.69%。通过晶界扩散DyFe使矫顽力增幅为22.40%。晶界扩散Dy后的磁钢在160℃/1h下,磁通不可逆损失从6.3%下降到1.1%,在180℃/2h下,磁通不可逆损失从22.6%下降到6.3%。在一定的热处理条件下,重稀土元素择优分布在主相和晶界相的交界处,这种改性的晶界结构和成分提高了各向异性场,大幅提高磁体的矫顽力和耐热性。     

DyAl合金薄膜在NdFeB基体上真空热扩渗行为的研究

采用直流(DC)磁控溅射的方法,在烧结NdFeB磁体表面制备了DyAl合金薄膜,镀膜样品经真空热扩渗(800℃×6h)和时效处理(900℃×2.5h+490℃×5h),研究了样品的微观结构组织与磁性,并对Dy、Al元素在基体中的真空热扩渗行为进行了探讨。结果表明,随着DyAl合金薄膜厚度的增加,磁体的内禀矫顽力Hcj相应提高,内禀矫顽力Hcj提高176kA/m(2.2kOe)。通过对样品微观组织结构观察发现,Dy和Al元素沿晶界富Nd相优先扩散,大量集中分布在主相晶粒表层和富Nd相交界处,不仅改善了晶界表面浸润性,也改变了主相晶粒表层合金成分和微结构,这种晶粒表面与晶界相的改性导致烧结NdFeB磁体的内禀矫顽力Hcj提高。     

晶界扩散Dy60Co35Ga5合金对烧结钕铁硼磁体 磁性能及热稳定性的影响

研究了晶界扩散Dy₆₀Co₃₅Ga₅合金对烧结钕铁硼磁体磁性能及其热稳定性的影响.随着扩散温度的升高,磁体的矫顽力（H_cj）呈现出先增加后减少的趋势,并在890 ℃扩散3 h,480 ℃回火5 h的工艺条件下,矫顽力达到较优,从1 209 kA/m提高到1 624 kA/m,磁体的剩磁只有轻微的下降,从1.38 T降低到1.32 T.高温下测试磁体的磁性能,原始磁体和890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的矫顽力都呈下降趋势,但晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的矫顽力在高温下要明显优于原始磁体.原始磁体及890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体在不同温度下保温2 h的不可逆磁通损失分别为63 %和45 %.且DSC结果显示,890 ℃晶界扩散Dy₆₀Co₃₅Ga₅合金磁体的居里温度（T_c）要明显高于原始磁体的居里温度,这表明晶界扩散磁体的热稳定性得到了很大的改善. XRD图谱显示,890 ℃晶界扩散磁体RE₂Fe₁₄B相的衍射峰较原始磁体向右偏移,说明Dy原子及Co原子少部分已进入主相晶粒.      

7055铝合金多级均匀化工艺研究

采用中频炉熔炼7055铝合金,用光学显微镜、扫描电镜、能谱仪和万能拉伸机等方法研究多级均匀化工艺对7055铝合金显微组织及力学性能的影响。结果表明：未经均匀化处理的7055铝合金铸锭存在着严重的组织偏析,合金经470℃×30 h单极均匀化处理后,晶界上的非平衡相有所减少,已形成不连续分布,成分偏析得到改善;在单极均匀化基础上增加410℃×4 h的中间保温,均匀化效果更好,非平衡相的溶解数量增多,晶界更为平直,且形状规整;而经250℃×4 h＋410℃×4 h＋470℃×30 h三级均匀化处理后,消除了铸锭晶界上的非平衡凝固共晶组织,晶界呈线条状。经时效处理后,其力学性能较优。     

烧结Nd-Fe-B磁体晶界扩散TbH2高温稳定性及其机理

采用涂敷方式,在烧结钕铁硼表面均匀涂敷TbH₂粉末,经过不同的扩散温度处理,制备出晶界扩散磁体。研究了晶界扩散TbH₂对烧结Nd-Fe-B磁体常温磁性能及高温稳定性的影响,并分析了磁体矫顽力提升的机理。常温磁性能研究表明,扩散磁体经过890 ℃+490 ℃工艺处理后性能达到最优,矫顽力从1 383 kA/m提升到1 988 kA/m。高温磁性能结果显示,扩散磁体200 ℃的矫顽力温度系数|β|比原始磁体降低0.032%/℃,磁通不可损失hirr比原始磁体降低21.47%,扩散TbH₂明显提高了烧结Nd-Fe-B磁体的热稳定性。分析得出,晶界扩散TbH₂磁体矫顽力提升的机理是Nd₂Fe₁₄B晶粒外延层形成了（Tb, Nd）₂Fe₁₄B核壳结构,提高了磁晶各向异性场;同时改善了磁体的微观组织结构,有效地隔绝了晶粒之间的磁交换耦合作用。      

(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.      

DyF3热扩渗技术提高NdFeB磁体矫顽力及其机理分析

以商业45H磁体为研究对象,用自制的DyF3涂料涂覆到磁体表面,进行热扩渗处理.通过热扩渗温度和时间的正交实验,确定了磁体的最佳热扩渗工艺为940℃×10h,磁体矫顽力从初始的1.39 MA/m提升至1.76MA/m,增幅高达26.6％.通过对磁体微观组织结构的分析,研究了重稀土元素Dy的热扩渗过程及磁体矫顽力提高机理...     

高Dy含量烧结Nd-Fe-B的晶界扩散处理研究

研究了晶界扩散处理对高Dy含量烧结Nd-Fe-B磁体性能和结构的影响。经蒸镀渗Dy晶界扩散处理,高Dy含量Nd-Fe-B磁体的矫顽力从1 713 kA/m提高至2 161 kA/m,而剩磁和最大磁能积基本没有下降,处理后磁体内Dy平均质量分数仅增加0.30%。不同深度片层分析表明,虽然磁体近表面片层比中心片层的Dy含量高,但是片层间矫顽力相差较少,而且所有片层的矫顽力均远高于未处理磁体片层的矫顽力。电子探针Dy元素面分布结果显示,在未处理高Dy含量磁体的晶界与主相中均存在Dy元素富集区且富集浓度较低,而经扩散处理后,晶界富Nd相中的Dy富集区浓度及所占比例明显提高;包括磁体芯部在内,磁体内大部分角隅处富Nd相内Dy含量明显增加,进一步提高了高Dy含量磁体内部各处的矫顽力。     

时效对NdFeB烧结磁体的矫顽力和显微组织的影响

本文主要研究了时效对ＮｄＦｅＢ烧结磁体的矫顽力和显微组织的影响。结果表明，６００℃左右的时效可显著提高烧结ＮｄＦｅＢ磁体的矫顽力。原因在于：①时效使主相晶界平直、规整，从而使反磁化畴难以形核。②晶界中的微粒相数量增多，强化了对晶界的钉扎。正是这两种因素的共同作用使得时效后磁体的矫顽力提高了。     

ECAP制备TWIP钢的力学性能研究

采用ECAP方法对TWIP钢(30Mn-3Si-3A1)试样进行一道次等径角挤压(ECAP)变形,对比研究原始态、一道次挤压态、ECAPlP+850℃×1h(空冷)处理和ECAPlP+1000℃×1h空冷处理后的微观结构及力学性能.试验结果表明:在变形过程中,形变孪晶的相互形变阻力和位错在形变孪晶界的大量塞积,使TWI...     

Effect of aluminum on microstructure and magnetic properties of sintered Nd-Fe-B magnets processed by grain boundary diffusion of Tb-Al

The grain boundary diffusion process(GBDP) of Tb can improve the coercivity of sintered Nd-Fe-B magnets.In this study,the effect of AI on the diffusion of Tb in the GBDP was investigated.The content of diffused Tb-Al was precisely controlled by adjusting the magnetron sputtering process.The Tb equivalent of Al was also studied.Results show that AI promotes the diffusion of Tb deeper into the magnet,reducing the thickness of the shell in the core-shell structure.This study is helpful for further ...     

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.     

晶界扩散中Tb对烧结NdFeB磁体微观组织和磁性能的影响

通过晶界扩散技术提升烧结钕铁硼(NdFeB)磁体矫顽力的方法已获得广泛应用,为了研究重稀土磁粉对磁体综合磁性能的影响,本文采用喷涂扩散的方法将重稀土Tb含量为6.0%(质量分数)的磁粉作为复合扩散源的一部分进行晶界扩散并制备了高性能烧结NdFeB磁体。结果表明,当主扩散源占比为60%(质量分数)时,Nd₄₀Tb₆₀对应扩散磁体的矫顽力最高达到21.52 kOe,矫顽力增幅明显。经过微观组织结构和XRD表征分析,重稀土元素Tb沿晶界相扩散进入磁体内部的同时发生了晶格取代反应,可在晶粒表层生成磁晶各向异性场更强的(Nd,Dy/Tb)₂Fe₁₄B硬磁相,显著增强了磁体矫顽力。当主扩散源占比为20%、40%和80%(质量分数)时,Nd₈₀Tb₂₀,Nd₆₀Tb₄₀和Nd₂₀Tb₈₀对应扩散磁体的矫顽力增幅较小,其中Nd₈₀Tb₂₀扩散...     

Improvement of microstructure and coercivity for Nd-Fe-B sintered magnets by boundary introducing low melting point alloys

Different from the grain boundary diffusion process(GBDP),which is suitable for modifying thin magnet,a green-pressing agents permeation process(GAPP) that uses low melting point alloys was applied to the Nd-Fe-B green compact with a thickness over 15 mm to reconstruct the boundary microstructure of a sintered Nd-Fe-B magnet.The coercivity increases from 12.3 kOe for the sample free of Pr_(80)Al_(20) to16.8 kOe for the sample with 2 wt% Pr_(80)Al_(20).By further increasing the Pr_(80)Al_(20) content to 3 wt%,the coercivity increases slightly,but the remanence and H_k/H_(cj) deteriorate obviously.The optimal comprehensive properties of H_(cj)=16.8 kOe,B_r=13.4 kG and H_k/H_(cj)=0.975 are obtained at 2 wt% Pr_(80)Al_(20),since matrix phase grains are separated by relatively continuous thin grain boundary layers,which weaken the magnetic coupling between adjacent grains.The coercivities of the samples from the GAPP that use2 wt% Pr_(80)Al_(20),Pr_(70)Al_(30) and Pr_(60)Tb_(20)Al_(20) alloys,respectively,can be enhanced to a large extent.However,the coercivity of the magnet reconstructed with Pr_(80)Al_(20) is lower than that of the sample with Pr_(60)Tb_(20)Al_(20) but is higher than that of the sample reconstructed with Pr_(70)Cu_(30) alloy.Moreover,the coercivity of the sample from the GAPP using 2 wt% Pr_(80)Al_(20) is much higher than that of the sample from the GBDP,which is due to a nearly uniform boundary microstructure from the surface to the interior of the thick magnet from the GAPP,thus providing new insights into the fabrication of thick and bulky permanent magnets with high coercivity.     

Magnetic properties and microstructures of terbium coated and grain boundary diffusion treated sintered Nd-Fe-B magnets by magnetron sputtering

Tb coating on the surface of commercial sintered Nd-Fe-B magnet was prepared by DC magnetron sputtering.The secondary heat treatment was used to regulate the microstructure for the enhancement of coercivity,namely diffusion treatment and annealing treatment.The coercivity increases significantly from 18.3 to 28.0 kOe,the remanence decreases slightly from 14.1 to 14.0 kGs,and the comprehensive magnetic properties are higher than 75(Hcj+(BH)_max=76.7).SEM results indicate that,on the one hand,950℃is the optimal diffusion temperature.Lower diffusion temperature results in insufficient diffusion of Tb element.Higher diffusion temperature can lead to the main phase grain growth,the decrease of Nd-rich phase,and forming holes in the magnet.On the other hand,500℃is the optimal annealing temperature.Lower annealing temperature can result in the reduction of Nd-rich phase.Higher annealing temperature can generate the non-defined Nd-rich thin layer between grains.     

Magnetic field stability of PrFeB magnets developed by GBD for cryogenic permanent magnet undulators

The magnetic field stability of the PrFeB magnets is one of the key points which affect its application in such devices as cryogenic permanent magnet undulators. In this study, the magnetic properties and microstructure of PrFeB magnets, which were developed by the grain boundary diffusion, were examined. The demagnetizing field distribution of the cryogenic permanent magnet undulator made using the PrFeB magnets was simulated by Radia, and the change mechanism of the irreversible demagnetization following treatments at high temperatures was experimentally studied. The results show that the intrinsic coercivity of the PrFeB magnets can be increased by diffusion of Tb. Meanwhile, the remanence of the magnets displays almost no loss, and the increasing range is closely related to the orientation thickness of the PrFeB magnet. Therefore, the PrFeB magnets developed using grain boundary diffusion are found to have extremely high comprehensive magnetic properties. The irreversible demagnetization of the PrFeB magnets developed by grain boundary diffusion for the CPMU is determined to be significantly improved following high-temperature treatments.     

Coercivity enhancement mechanism of grain boundary diffused Nd-Fe-B sintered magnets by magnetic domain evolution observation

The grain boundary diffusion(GBD) technology was used to prepare high performance Nd-Fe-B sintered magnets by NdH_3 and TbH_3 nanoparticle diffusion.The factors affecting the coercivity of GBD magnets include distribution of rare earth rich grain boundary phase and substitution of the heavy rare earth.In order to distinguish the influence of various factors on the coercivity,the microstructure and magnetic domain evolution of the original,reference,Nd-diffused,and Tb-diffused magnets were analyzed.The core-shell structure formed by heavy rare earth substitution is the main factor of coercivity enhancement,and it can transform the magnetic domain reversal mode from easy-nucleation(EN) to difficultnucleation(DN).With increasing the diffusion depth,the shell of the core-shell structure gradually becomes thinner,DN grains gradually decrease while the EN grains gradually increase,indicating that the magnetic domain reversal mode is directly related to the core-shell structure.     

Effects of grain boundary diffusion process on magnetic properties enhancement and microstructure evolution of hot-deformed Nd-Fe-B magnets

Grain boundary diffusion(GBD) process is an important approach for producing Nd-Fe-B magnets with high coercivity and high thermal stability.The GBD for hot-deformed Nd-Fe-B magnets with nanocrystalline micro structure is more complicated compared to sintered magnets.Here,we investigated the effects of different GBD methods,i.e.,intergranular addition(in-situ GBD 1#),in-situ GBD from magnet surface during hot pressing and hot deformation(in-situ GBD 2#),and conventional GBD,on the magnetic prope...