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Journal Article

Formation of Bi2Ir nanoparticles in a microwave-assisted polyol process revealing the suboxide Bi4Ir2O

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Ruck,  Michael
Michael Ruck, Max Planck Fellow, Max Planck Institute for Chemical Physics of Solids, Max Planck Society;

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Citation

Smuda, M., Finzel, K., Hantusch, M., Stroeh, J., Pienack, N., Khadiev, A., et al. (2021). Formation of Bi2Ir nanoparticles in a microwave-assisted polyol process revealing the suboxide Bi4Ir2O. Dalton Transactions, 50(47), 17665-17674. doi:10.1039/d1dt03199f.


Cite as: https://hdl.handle.net/21.11116/0000-0009-9F8A-9
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(NO3)(3) and Ir(OAc)(3), the new suboxide Bi4Ir2O forms as an intermediate phase at about 160 degrees C. Its structure was determined by a combination of PXRD and quantum-chemical calculations. Bi4Ir2O decomposes in vacuum at about 250 degrees C and is reduced to Bi2Ir by hydrogen at 150 degrees C. At about 240 degrees C, the polyol process leads to the immediate reduction of the two metal-containing precursors and crystallization of Bi2Ir nanoparticles.