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

目的是：持久性增强的磁铁从硬和软磁性相位的两个阶段纳米结构中制造出来，可以由任何熔融旋转或机械合金制备。我们先前的工作展示了两个阶段的混合物也可以被氢化分散分解重组（HDDR）处理的Sm D23 Y D2（Fe，V）Y D229 Y D2到TbCu D27 Y D2类型和αFe（V）相位，其中展示了大约0.6 MAm Y D1-1 Y D1 （7 kOe）后的协同作用。However，HDDR处理材料的颗粒大小（~ 300纳米）通常比强度大，因为它需要增强持久性：软颗粒理想上应该是10 - 20纳米。Cohas的补充显示出在减少重组温度和颗粒大小的HDDR治疗样品中具有有效性。因此，该工作的目标是研究Co对分散和重组动力学的影响（Fe，V）Wei D229 Wei D2（Fe，V）Wei D229 Wei D2，并试图减少其影响。 ... More e grain size of the grain size of the grain d2 a grain d2 Fe（Co，V）/TbCu grain D27 grain D27 grain D2 type phase mixture.实验过程： Alloys of smy D29.4 grain d2 Fe y d284.6-x grain d2Coxv grain D26.0 grain D2 （X = 0、10、20和30）， were induction melted from high purity elements， under an aratmosphere，然后在1150℃下均匀化20小时。X-ray Diffraction （XRD）分析显示了alloys were near single phase Sm D23 y D2（Fe， Co， V）y D229 y D2与αFe（Co， V）的小剂量。均匀允许将颗粒放入粉末中，将颗粒尺寸缩小到小于63微米，并将其压入绿色伴侣。样品在分化反应的不同阶段产生，在620 - 700 ° C之间加热到温度，然后一小时后，在氢中快速冷却。HDDR样品在590 - 750 ° C之间加热到不成比例的样品后获得，然后在10分钟- 12小时后快速冷却真空下。一些HDDR样本在560℃下被点燃，在4小时内D23）D2，然后地面进入粉末，其中一个固体填充物混合在1.0 MA D2 m-1 D2 （12 kOe）的磁场中。magnetic properties were measured using a vibrating sample magnetometer （VSM）。传输电子显微镜（TEM）的样本由离子铣削来思考。结果：随着钴的添加，铝合金Sm D29.4 Fe D284.6-X Y D2CoxV Y D26.0 Y D2 （X = 0、10、20和30）增加，并重新组合温度降低。This shows that cobalt stabilizes the smyy D23 ye D2（Fe， Co， V）y D229 ye D2 phase with respect to disproportionation in hydrogen， and increases the recombination in αFe（Co， V） and TbCu D27 ye D2 type phase. With TEM [近似等于] 5 nm直径柱是可见的，谁相信是SmHs。在630 ° C的1小时内发现了约50 - 100纳米的尺寸，在30%的Co样品中重新组合。在添加到αFe（Co， V）和TbCuy D27型D2型相位中， XRD还显示了在高钴含量和低温度下仍未识别的相位的存在，其中出现了对磁性性能的不利影响，在夜间后。Less（低）

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