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Synthesis of nanocrystalline filled skutterudites by mechanical alloying

机译：机械合金化合成纳米晶体填充薄岩

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We report on the preparation of nanocrystalline filled skutterudites in the series Ce{sub}yFe{sub}(4-x)Co{sub}xSb{sub}12 by mechanical alloying. X-ray diffraction and energy dispersive X-ray spectroscopy reveal that skutterudites can be prepared with an homogeneity range larger than what can be obtained by powder metallurgy (PM). Interestingly, no after-milling thermal treatment is required to prepare essentially single phase samples (～90-95%). This is an important difference with skutterudites prepared by PM which only form after long term annealing below the peritectic decomposition temperature. Differential thermal analysis shows that grain growth occurs above ～350°C and that the peritectic decomposition temperature is similar to PM-^s(i.e. 750°C for x = 1). Grain sizes are in the 12-30 nm range as deduced from Rietveld refinements of X-ray diffraction data and Scanning Electron Microscopy. Cerium is trivalent in nanocrystalline filled skutterudites, as it is in samples prepared by PM. Both p-type and n-type skutterudites can be obtained but values of the Seebeck coefficient are of the same order of magnitude as in PM samples only for p-type skutterudites.
机译：通过机械合金化报告在CE {Sub} YFE {sub}（4-x）Co {Sub} 12系列中的纳米晶体填充Skutterudites的制备。 X射线衍射和能量分散X射线光谱揭示了斯皮特拉迪斯可以使用大于通过粉末冶金（PM）可以获得的均匀性范围来制备。有趣的是，不需要碾磨后的热处理来制备基本单相样品（〜90-95％）。这是PM由PM准备的Skutturedites的重要区别，该斯皮特拉迪斯在短期内退火后，在晶间分解温度下方的长期退火。差分热分析表明，谷物生长发生在〜350℃以上，并且包晶分解温度类似于PM-^ S（即750℃，X = 1）。从X射线衍射数据和扫描电子显微镜的RIETVELDETEMETEMENT中推断出12-30nm系列。铈是纳米晶体填充斯皮特拉迪斯的三价，因为它在PM制备的样品中。可以获得p型和n型Skutterudites两者，但塞贝克系数的值与P型Skuttudites的PM样本中的峰值相同。

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