采用电弧熔炼和退火的方法,成功地制备了Mn3+xSn1-x(x=0.1,0.05,0)系列样品。采用热重-热扫描(TG-DSC)研究了Mn3.1Sn0.9的吸氮峰,并成功氮化出Mn3.1Sn0.9N化合物。X射线衍射,扫描电镜和能谱X射线分析证明Mn3.1Sn0.9与Mn3.05Sn0.95均为Mn3Sn单相。而Mn3.0Sn1.0样品为Mn1.77Sn与Mn3Sn两相共存。在N2气氛下Mn3.1Sn0.9的TG-DSC曲线显示,在1151K和1267K出现2个吸氮峰。在1151K对Mn3.1Sn0.9渗氮得到Mn3.1Sn0.9N单相。Mn3.1Sn0.9与Mn3.1Sn0.9N化合物的结构相关,但各自的Mn原子间距差别明显。在Mn3.1Sn0.9N的八面体间隙位引入N原子,通过相邻2层的间隙或者同一层的间隙才能进入体心位。这也说明在TG-DSC曲线上出现2个连续的、相隔不远的吸氮峰的原因。实验上也证明在2个温度渗氮得到的是相同的化合物。
By means of magneto-controlled arc furnace followed by annealling, Mn3+xSn1-x ( x= 0. 1,0.05,0 ) compounds were successfully prepared. TG-DSC reveals both nitrogen-absorption peaks on the curve of Mn3.1Sn0.9, and Mn3.1 Sn0. 9 N compound was produced. By means of X-ray diffraction, SEM and EDS X-ray analysis, both Mn3.1Sn0.9 and Mn3.05Sn0.05 compounds exhibit single phase, while Mn3. 0Sn1. 0 sample displays a coexistence of Mn1. 77Sn and Mn3Sn phases. The TG-DSC curves reveal, double nitrogen-absorption peaks occur at 1 151 and 1 267 K respectively. By nitrogenation of Mn3.1Sn0.9, Mn3.1 Sn0.9N compound can be produced at 1 151 or 1 267 K. Despite the correlation between Mn3.1Sn0.9 and Mn3.1Sn0.9N, the distance between Mn atoms of them is different. In order to introduce N atom into the interstices of Mn3.1Sn0.9, N atoms enter into either the interstices between the nearest and second nearest or the interstice of bottom cells of Mn3.1 Sn0.9, which illustrates the presence of both nitrogen-absorption peaks on the TG-DSC curves. Moreover, the experience also confirms our analysis.