Home > Publications database > Formation of Bi$_2$Ir nanoparticles in a microwave-assisted polyol process revealing the suboxide Bi$_4$Ir$_2$O |
Journal Article | PUBDB-2021-05068 |
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2021
Soc.
London
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Please use a persistent id in citations: doi:10.1039/D1DT03199F doi:10.3204/PUBDB-2021-05068
Abstract: Intermetallic phases are usually obtained by crystallization from the melt. However, phases containing elements with widely different melting and boiling points, as well as nanoparticles, which provide a high specific surface area, are hardly accessible via such a high-temperature process. The polyol process is one option to circumvent these obstacles by using a solution-based approach at moderate temperatures. In this study, the formation of Bi2Ir nanoparticles in a microwave-assisted polyol process was investigated. Solutions were analyzed using UV–Vis spectroscopy and the reaction was tracked with synchrotron-based in situ powder X-ray diffraction (PXRD). The products were characterized by PXRD and high-resolution transmission electron microscopy. Starting from Bi(NO$_3$)$_3$ and Ir(OAc)$_3$, the new suboxide Bi$_4$Ir$_2$O forms as an intermediate phase at about 160 °C. Its structure was determined by a combination of PXRD and quantum-chemical calculations. Bi$_4$Ir$_2$O decomposes in vacuum at about 250 °C and is reduced to Bi$_2$Ir by hydrogen at 150 °C. At about 240 °C, the polyol process leads to the immediate reduction of the two metal-containing precursors and crystallization of Bi2Ir nanoparticles.
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