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Reaction mechanism and thermoelectric properties of In0·22Co4Sb12 prepared by magnesiothermy
Materials Today Chemistry ( IF 7.3 ) Pub Date : 2020-06-01 , DOI: 10.1016/j.mtchem.2019.100223
S. Le Tonquesse , É. Alleno , V. Demange , C. Prestipino , O. Rouleau , M. Pasturel

Abstract The magnesioreduction synthesis of In0·22Co4Sb12 with high In rattler concentration from Sb2O4 and In-doped Co3O4 precursors is reported. This process directly yields a submicronic powder in a single step of 96 h at 810 K. The reaction mechanism has been investigated by stopping the reaction every 12 h and quantifying the existing phases by X-ray diffraction and Rietveld refinements. The precursors are first reduced in CoO and Sb2O3 lower oxides, then form CoSb2O6 and CoSb2O4 intermediates which are finally reduced in InxCo4Sb12. A powder with 350 nm average size and mostly composed of In-filled skutterudite phase with composition close to In0·17Co4Sb12 is obtained. Upon spark plasma sintering, small residual amount of InSb reacts with the skutterudite matrix to form a single-phase densified pellet with composition close to In0·22Co4Sb12. The resulting densified material with 1.8 μm average grain size shows a figure of merit ZTmax of 0.95 at 750 K.

中文翻译:

镁热法制备In0·22Co4Sb12的反应机理及热电性能

摘要 报道了用 Sb2O4 和掺 In 的 Co3O4 前驱体镁还原合成具有高 In 响尾蛇浓度的 In0·22Co4Sb12。该过程在 810 K 下 96 小时的单个步骤中直接产生亚微米粉末。通过每 12 小时停止反应并通过 X 射线衍射和 Rietveld 精修量化现有相来研究反应机理。前体首先在 CoO 和 Sb2O3 低级氧化物中还原,然后形成 CoSb2O6 和 CoSb2O4 中间体,最终在 InxCo4Sb12 中还原。获得平均尺寸为 350 nm 且主要由成分接近 In0·17Co4Sb12 的填充方钴矿相组成的粉末。放电等离子烧结时,少量残留的 InSb 与方钴矿基体反应,形成成分接近 In0·22Co4Sb12 的单相致密球团。
更新日期:2020-06-01
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