TMA Study on Phase Evolution During Hydrogen-assisted Disproportionation of Nd-Fe-B Alloy

Phase evolution during the hydrogen-assisted disproportionation of $Nd_{12.5}Fe_{80.6}B_{6.4}Ga_{0.3}Nb_{0.2}$ alloy was investigated mainly by using a magnetic balance-type thermomagnetic analyser (TMA). In order to avoid any undesirable phase change in the course of heating for TMA, a swift TMA technique with very high heating rate (around 2 min to reach $800^{\circ}C$ from room temperature) was adopted. The hydrided $Nd_{12.5}Fe_{80.6}B_{6.4}Ga_{0.3}Nb_{0.2}$ alloy started to be disproportionated in hydrogen from around $600^{\circ}C$, and the alloy after the early disproportionation (from 600 to $660^{\circ}C$) has been partially disproportionated. The partially disproportionated alloy consisted of a mixture of $NdH_x$, $Fe_3B$, ${\alpha}$-Fe, and the remaining undisproportionated $Nd_2Fe_{14}BH_x$-phase. During the subsequent heating to $800^{\circ}C$ in hydrogen, two additional phases of $Fe_{23}B_6$ and $Fe_2B$ were formed, and the material consisted of a mixture of $NdH_x$, $Fe_{23}B_6$, $Fe_3B$, $Fe_2B$, and ${\alpha}$-Fe phases. During the subsequent isothermal holding at $800^{\circ}C$ for 1 hour, the phase constitution was further changed, and one additional unknown magnetic phase was formed. Eventually, the fully disproportionated $Nd_{12.5}Fe_{80.6}B_{6.4}Ga_{0.3}Nb_{0.2}$ alloy consisted of $NdH_x$, $Fe_{23}B_6$, $Fe_3B$, $Fe_2B$, ${\alpha}$-Fe, and one additional unknown magnetic phase.