Low-temperature solution synthesis of nanocrystalline binary intermetallic compounds using the polyol process
Low-temperature solution synthesis of nanocrystalline binary intermetallic compounds using the polyol process
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DOI：
10.1021/cm0520113
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发表时间：
2005-12-27
影响因子：
8.6
通讯作者：
Schaak, RE
中科院分区：
文献类型：
--
作者：
Cable, RE;Schaak, RE
采用改进的多元醇工艺，以四甘醇为溶剂，在低温下由金属盐前体合成了纳米晶金属间化合物粉末。该溶液路线已在 M-Sn（M = Ag、Au、Co、Cu、Fe、Ni）、Pt-M'（M' = Bi、Pb、Sb、Sn）和 Co-Sb 双金属体系中产生了几种纯相化合物。在Co-Sb体系中，通过控制初始金属浓度和反应温度可以选择性地生产CoSb和CoSb3。 Co-Sn 和 Cu-Sn 体系可以在单个反应过程中根据温度选择性地形成 Co3Sn2 与 CoSn 和 Cu6Sn5 与 Cu41Sn11。这些结果证明了这些金属间化合物系统中晶体结构的动力学控制。可以在不同的时刻监测反应进程。通过 XRD 分析时间和温度，深入了解反应路径。 TEM 显微照片显示，M-Sn 系统的粒径范围为 5 至 50 nm，而 Pt-M' 系统的粒径范围为 10 至 100 nm。 SEM 显微照片显示这些颗粒聚集形成密集的 100-200 nm 簇。 DSC 数据表明，使用多元醇工艺合成的金属间化合物在接近散装粉末预期温度的温度下表现出有序-无序相变。纳米晶体粉末可在溶液中再分散，初步实验表明它们可以通过纳米级模具进行模板化，从而实现基于溶液的材料加工应用。
Nanocrystalline intermetallic powders have been synthesized from metal salt precursors at low temperatures using a modified polyol process with tetraethylene glycol as the solvent. This solution route has yielded several phase-pure compounds in the M-Sn (M = Ag, Au, Co, Cu, Fe, Ni), Pt-M', (M' = Bi, Pb, Sb, Sn), and Co-Sb bimetallic systems. In the Co-Sb system, CoSb and CoSb3 can be selectively produced by controlling the initial metal concentrations and the reaction temperature. The Co-Sn and Cu-Sn systems can selectively form Co3Sn2 Vs CoSn and Cu6Sn5 VS Cu41Sn11 during a single reaction as a function of temperature. These results demonstrate kinetic control over crystal structure in these intermetallic systems. The reaction progress may be monitored at different. times and temperatures by XRD, giving insight into the reaction pathways. TEM micrographs show that the particle sizes in the M-Sn systems range from 5 to 50 nm, while the Pt-M' systems range from 10 to 100 nm. SEM micrographs show that these particles aggregate to form densely packed 100-200 nm clusters. DSC data show that the intermetallics synthesized using the polyol process exhibit order-disorder phase transitions at temperatures near those expected for bulk powders. The nanocrystalline powders are redispersible in Solution, and preliminary experiments have shown that they may be templated by nanoscale molds, allowing for solution-based materials processing applications.