Comparison between different techniques for obtaining anisotropic Nd–Fe–B hard magnetic powders by the HDDR process

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The method for obtaining anisotropic hard magnetic Nd2Fe14B powders by the process Hydrogenation–Disproportionation–Desorption–Recombination (HDDR process) Nd–Fe–B type alloy with high content of Nd has been considered in this study. Two different types of HDDR (dynamic and solid) process have been studied. The dependence of magnetic hysteresis properties on hydrogen pressure and its pumping rate at the disproportionation stage is shown. It is found that a solid HDDR makes it possible to obtain powders with higher coercivity and the hysteresis loop rectangularity than a dynamic HDDR.

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作者简介

I. Ivanov

The Institute of Natural Sciences and Mathematics, Ural Federal University; Institute of Metal Physics, Ural Branch, Russian Academy of Sciences

编辑信件的主要联系方式.
Email: ilya.ivanov@urfu.ru
俄罗斯联邦, Ekaterinburg, 620000; Ekaterinburg, 620108

A. Golubiatnikova

The Institute of Natural Sciences and Mathematics, Ural Federal University

Email: ilya.ivanov@urfu.ru
俄罗斯联邦, Ekaterinburg, 620000

N. Selezneva

The Institute of Natural Sciences and Mathematics, Ural Federal University

Email: ilya.ivanov@urfu.ru
俄罗斯联邦, Ekaterinburg, 620000

A. Protasov

Institute of Metal Physics, Ural Branch, Russian Academy of Sciences

Email: ilya.ivanov@urfu.ru
俄罗斯联邦, Ekaterinburg, 620108

A. Volegov

The Institute of Natural Sciences and Mathematics, Ural Federal University

Email: ilya.ivanov@urfu.ru
Ekaterinburg, 620000

参考

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2. Fig. 1. Schematic diagram of the structural changes during the HDDR process: (a) initial alloy with large Nd2Fe14B and Nd grains; (b) hydrogen penetration into the alloy along the grain boundary. Structural changes during d-HDDR: (c) hydrogenation of Nd2Fe14B grains occurs locally and propagates as a front; (d) thin NdH2 and Fe2B plates combined into small colonies are formed as a result of the early stage of HD. Structural changes during s-HDDR: (d) hydrogen penetration occurs almost along the entire grain boundary; (e) thickened plates forming large colonies are formed at the early stage of HD.

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3. Fig. 2. Formation of spherical grains of NdH2 and Fe2B during the end of the HD stage (a); formation of a submicron structure within the boundaries of the initial Nd2Fe14B grain as a result of the HDDR process (b).

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4. Fig. 3. Schematic diagram of d-HDDR with preliminary Hydrogen Decripitation (HDe) reaction (a); Tdisp – disproportionation onset temperature. Schematic diagram of s-HDDR with preliminary HDe reaction (b).

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5. Fig. 4. Diffraction patterns of d- and s-HDDR powders obtained at different hydrogen pressures (unmarked reflections correspond to the main phase Nd2Fe14B).

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6. Fig. 5. Limiting magnetic hysteresis loops of d-HDDR powders obtained at a hydrogen pressure of (a) 20 kPa and (b) 30 kPa. (c, d) – actual schemes of the HD stages during an increase in temperature from T1 to T2 and the beginning of the DR stages of d-HDDR processes: I – the region where hydrogen was not additionally pumped out of the ampoule and the areas of decreasing pressure are due to sorption; II – the region where premature hydrogen desorption occurs as a result of thermodynamic equilibrium violation during heating (areas of increasing pressure), hydrogen is pumped out using a vacuum post (vertical sections); III – pumping out of the ampoule (DR stage); 1 – cooling as a result of desorption starting due to the evacuation of the ampoule, 2 – the area of ​​slow pumping of hydrogen into the ampoule.

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7. Fig. 6. Typical appearance of the alloy heating process in a hydrogen/argon environment and the HD stage at the moment of hydrogen pumping during s-HDDR. The dashed line highlights the boundaries of the sections where the following are typical: 1 – hydrogen desorption; 2 – absorption of desorbed hydrogen; 3, 5 – weak absorption of hydrogen during the HD stage; 4 – active sorption during the HD stage.

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8. Fig. 7. Limiting magnetic hysteresis loops measured with the texture axis oriented along the applied field for s-HDDR powders synthesized at hydrogen pressures of 90 and 110 kPa.

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