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研究了Fe置换CoSb3基Skutterudite化合物Co4-xFexSb12(x≤1)的机械合金化及其制备工艺。在研究的成分范围内,所有的成分显示出相似的机械合金化动力学过程,初期Skutterudite相比(Co/Fe)Sb2相更易于形成,但随球磨时间进一步延长,(Co/Fe)Sb2相逐渐成为最强相。通过机械合金化不能得到单相的Skutterudite结构。球磨10小时的粉末经过热压成形后,大部分已转变为Skutterudite相,但仍有少量残存的Sb杂质。热压后进一步在650℃退火48小时后,得到了基本为单相的Skutterudite结构化合物Co4-xFexSb12(x≤0.65),且x=0.65时基本达到了Fe的置换固溶度。
The mechanical alloying of Fe-substituted CoSb3-based Skutterudite compound Co4-xFexSb12 (x≤1) and its preparation process were studied. Within the studied composition range, all the components showed a similar mechanical alloying kinetics. The initial phase of Skutterudite was easier to form than the (Co / Fe) Sb2 phase, but with the further increase of milling time, the (Co / Fe) Gradually become the strongest phase. Single-phase Skutterudite structures can not be obtained by mechanical alloying. After 10 hours of powder milling, most of the powder has been transformed into Skutterudite after hot press forming, but there is still a small amount of residual Sb impurities. After hot pressing and further annealing at 650 ° C for 48 hours, a substantially single-phase structure of the compound Sk4-xFexSb12 (x≤0.65) was obtained, and the substitutional solid solubility of Fe was achieved at x = 0.65.