Orefice Martina, Xu Xuan, Žužek Rožman Kristina, Šturm Sašo, Binnemans Koen
KU Leuven, Department of Chemistry, Celestijnenlaan 200F, P.O. Box 2404, B-3001 Heverlee (Belgium).
Jožef Stefan Institute (JSI), Department for Nanostructured Materials K7, Jamova Cesta 39, SI-1000 Ljubljana (Slovenia).
Data Brief. 2020 Aug 20;32:106203. doi: 10.1016/j.dib.2020.106203. eCollection 2020 Oct.
Three phases can be distinguished in Nd‒Fe‒B permanent magnets: a NdFeB matrix grain phase, a Nd-rich grain boundary phase and a Nd-oxide phases. Common reaction models for leaching, such as the shrinking-particle model, cannot simply be applied to composite Nd‒Fe‒B permanent magnets because of the different chemical reactivities of the crystalline phases mentioned above. Etching the surface of a Nd‒Fe‒B magnet to expose its microstructure to electron microscopy is a necessary practice to correlate the microstructure itself to the specific properties of the magnets. Aqueous solutions of mineral acids are often used for etching purposes. However, these solutions are too low viscous to easily control the etching front and they show little selectivity in the etching process. In our work, the ionic liquid Cyphos IL 101 was used to etch bulk magnets instead of aqueous HCl solutions. The bulk Nd‒Fe‒B magnets were first polished, then exposed to a solution of 3 M HCl in Cyphos IL 101 for different times and at different temperatures. Afterwards, the etched Nd‒Fe‒B magnets were washed with ethanol and acetone. The results were examined via scanning-electron microscopy and image analysis. A commercial software, ImageJ®, was employed for image analysis. The latter technique was used to correlate the etched area (%area) or the grain and oxide size to the etching temperature or the etching time. The grain or the oxide size were calculated as Feret diameter. Image analysis revealed to be a necessary tool to support and correct the findings first suggested by the simple scanning-electron microscopy. The data presented in this article might be reused to corroborate a new reactivity order of the three Nd‒Fe‒B phases, different from that traditionally reported in literature, which is - from the most to the least reactive - grain boundary > oxides > the NdFeB grain phase.
钕铁硼基体晶粒相、富钕晶界相和钕氧化物相。常见的浸出反应模型,如收缩颗粒模型,由于上述晶相的化学反应性不同,不能简单地应用于复合钕铁硼永磁体。蚀刻钕铁硼磁体表面以将其微观结构暴露于电子显微镜下,是将微观结构本身与磁体的特定性能相关联的必要操作。无机酸水溶液常被用于蚀刻目的。然而,这些溶液粘度太低,难以轻松控制蚀刻前沿,并且在蚀刻过程中选择性很小。在我们的工作中,离子液体Cyphos IL 101被用于蚀刻块状磁体,而不是盐酸水溶液。块状钕铁硼磁体首先进行抛光,然后在不同温度下于Cyphos IL 101中的3 M盐酸溶液中暴露不同时间。之后,将蚀刻后的钕铁硼磁体用乙醇和丙酮洗涤。通过扫描电子显微镜和图像分析检查结果。使用商业软件ImageJ®进行图像分析。后一种技术用于将蚀刻面积(%面积)或晶粒和氧化物尺寸与蚀刻温度或蚀刻时间相关联。晶粒或氧化物尺寸计算为费雷特直径。图像分析被证明是支持和修正最初由简单扫描电子显微镜提出的结果的必要工具。本文所呈现的数据可能会被重新用于证实钕铁硼三相的一种新的反应活性顺序,该顺序与传统文献报道的不同,即从反应活性最高到最低依次为:晶界>氧化物>钕铁硼晶粒相。