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Production of Rare Earth-Fe Bonded Magnet Powders with High Remanence Utilizing Gas Reaction

利用气体反应生产高剩磁稀土铁粘结磁粉

基本信息

批准号：
10450252
负责人：
SUGIMOTO Satoshi
金额：
$ 4.1万
依托单位：
TOHOKU UNIVERSITY
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
1998
资助国家：
日本
起止时间：
1998 至 1999
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-10450252/
关键词：
HDDR 3:29 phase permanent magnets disproportionation TbCuィイD27ィエD2 phase

项目摘要

Purpose : Remanence enhanced magnets made from a 2 phase nanostructure of hard and soft magnetic phases, can be prepared by either melt spinning or by mechanical alloying. Our previous work has shown that a 2 phase mixture can also be obtained by the Hydrogenation Disproportionation Desorption Recombination (HDDR) processing of SmィイD23ィエD2(Fe,V)ィイD229ィエD2 into TbCuィイD27ィエD2 type and αFe(V) phases, which exhibits coercivities of about 0.6 MAmィイD1-1ィエD1 (7 kOe) after nitriding. However, the grain size of HDDR processed materials (〜300 nm) is typically an order of magnitude larger than that necessary for remanence enhancement to occur : the soft grains should ideally be 10 - 20 nm. The addition of Co has been shown to be effective in reducing the recombination temperature and grain size of HDDR treated samples. Therefore, the aim of this work was to investigate the effect of Co on the disproportionation and recombination kinetics of SmィイD23ィエD2(Fe,V)ィイD229ィエD2, and to attempt to reduce th … More e grain size of the ィイD2aィエD2Fe(Co,V)/TbCuィイD27ィエD2 type phase mixture.Experimental Procedure : Alloys of SmィイD29.4ィエD2FeィイD284.6-XィエD2CoxVィイD26.0ィエD2 (X = 0, 10, 20 and 30), were induction melted from high purity elements, under an Ar atmosphere, and then homogenized at 1150℃ for 20 hours. X-ray diffraction (XRD) analysis showed that the alloys were near single phase SmィイD23ィエD2(Fe, Co, V)ィイD229ィエD2 with a small amount of αFe(Co, V). The homogenized allows were ground into powders, sieved to a particle size less than 63μm, and pressed into green compacts. Samples were obtained at different stages of the disproportionation reaction, by heating under hydrogen to temperatures between 620 - 700℃, and then after 1 hour, cooling rapidly in hydrogen. HDDR samples were obtained by heating the disproportionated samples under vacuum to temperatures between 590 - 750℃ ; and then after 10 min - 12 hours, cooling rapidly under vacuum. Some of the HDDR samples were then nitrided at 560℃ for 4 hours ィイD23)ィエD2, then ground into powder, which was mixed with molten paraffin that solidified within a magnetic field of 1.0 MAィイD2m-1ィエD2 (12 kOe). The magnetic properties were measured using a vibrating sample magnetometer (VSM). Samples for transmission electron microscopy (TEM) were thinned by ion milling.Results: With the addition of cobalt, the disproportionation temperature of the alloys SmィイD29.4ィエD2FeィイD284.6-XィエD2CoxVィイD26.0ィエD2 (X = 0, 10, 20 and 30) increased, and the recombination temperature decreased. This shows that cobalt stabilizes the SmィイD23ィエD2(Fe, Co, V)ィイD229ィエD2 phase with respect to disproportionation in hydrogen, and increases the rate of the recombination into αFe(Co, V) and TbCuィイD27ィエD2 type phases. With TEM【approximately equal】5 nm diameter rods were observed, which are believed to be SmHs. Grain about 50 - 100 nm in size were found in a 30% Co sample recombined at 630℃ for 1 hour. In addition to αFe(Co, V) and TbCuィイD27ィエD2 type phases, XRD also showed the presence of a yet unidentified phase that forms at high Co contents and low temperature, which appeared to have an adverse effect on the magnetic properties, after nitriding. Less

目的：利用软硬两相纳米结构制备剩磁增强磁体，可采用熔体纺丝或机械合金化制备剩磁增强磁体。我们之前的研究表明,一个两阶段混合也可以通过加氢歧化解吸重组(HDDR)处理的Smィイc15ィエD2(铁、V)ィイD229ィエD2成TbCuィイD27ィエD2类型和α铁(V)阶段,展品矫顽力的约0.6老妈ィイD1-1ィエD1氮化后(7 kOe)。然而，HDDR加工材料的晶粒尺寸（~ 300 nm）通常比发生剩余物增强所需的晶粒尺寸大一个数量级：理想的软晶粒尺寸应为10 - 20 nm。Co的加入可以有效降低HDDR处理样品的复合温度和晶粒尺寸。因此,这项工作的目的是调查公司对Sm的歧化和复合动力学ィイc15ィエD2(铁、V)ィイD229ィエD2,并试图减少th ... 更多的e粒度ィイD2aィエD2Fe(公司,V) / TbCuィイD27ィエD2型相混合。实验过程:合金的SmィイD29.4ィエD2FeィイD284.6-XィエD2CoxVィイD26.0ィエD2 (X = 0、10、20和30),从高纯度元素感应熔化,在基于“增大化现实”技术的氛围,然后在1150℃均质20小时。x射线衍射（XRD）分析表明，合金为接近单相的Sm γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ。将均质化后的颗粒磨成粉末，筛分至粒径小于63μm，然后压成绿色粉饼。在歧化反应的不同阶段，将样品在氢气下加热至620 - 700℃，然后在氢气中快速冷却1小时。歧化后的HDDR样品在真空下加热至590 ~ 750℃；然后在10分钟- 12小时后，在真空下快速冷却。然后将部分HDDR样品在560℃下氮化4小时，再研磨成粉末，与熔融石蜡混合，在1.0 MA的磁场下固化。用振动样品磁强计（VSM）测量了其磁性能。透射电子显微镜（TEM）用离子磨薄样品。结果：随着钴的加入，合金的歧化温度（X = 0、10、20、30）升高，复合温度降低；结果表明，在氢的歧化作用下，钴稳定了Sm γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ γ。透射电镜（TEM）观察到直径约为5 nm的棒状物，认为是SmHs。30% Co样品在630℃下复合1小时，晶粒尺寸约为50 ~ 100 nm。除了α铁(公司,V)和TbCuィイD27ィエD2型阶段,XRD显示未知的阶段的存在形式和低温高有限公司内容,似乎在磁特性有不利影响,氮化后。少