Synthesis of rare-earth metal and rare-earth metal-fluoride nanoparticles in 
ionic liquids and propylene carbonate

Siebels, Marvin; Mai, Lukas; Schmolke, Laura; Schütte, Kai; Barthel, Juri; Yue, Junpei; Thomas, Jörg; Smarsly, Bernd M.; Devi, Anjana; Fischer, Roland A.; Janiak, Christoph

doi:10.3762/bjnano.9.180

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Synthesis of rare-earth metal and rare-earth metal-fluoride nanoparticles in ionic liquids and propylene carbonate

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Thomas, Jörg
Structure and Nano-/ Micromechanics of Materials, Max-Planck-Institut für Eisenforschung GmbH, Max Planck Society;

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Citation

Siebels, M., Mai, L., Schmolke, L., Schütte, K., Barthel, J., Yue, J., et al. (2018). Synthesis of rare-earth metal and rare-earth metal-fluoride nanoparticles in ionic liquids and propylene carbonate. Beilstein Journal of Nanotechnology, 9(1), 1881-1894. doi:10.3762/bjnano.9.180.

Cite as: https://hdl.handle.net/21.11116/0000-0001-E84C-5

Abstract

Decomposition of rare-earth tris(N, N'-diisopropyl-2-methylamidinato)metal(III) complexes [RE(MeC(N(iPr)2))3] (RE(amd)3; RE = Pr(III), Gd(III), Er(III)) and tris(2,2,6,6-tetramethyl-3,5-heptanedionato)europium(III) (Eu(dpm)3) induced by microwave heating in the ionic liquids (ILs) 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([BMIm][NTf2]) and in propylene carbonate (PC) yield oxide-free rare-earth metal nanoparticles (RE-NPs) in [BMIm][NTf2] and PC for RE = Pr, Gd and Er or rare-earth metal-fluoride nanoparticles (REF3-NPs) in the fluoridedonating IL [BMIm][BF4] for RE = Pr, Eu, Gd and Er. The crystalline phases and the absence of significant oxide impurities in RE-NPs and REF3-NPs were verified by powder X-ray diffraction (PXRD), selected area electron diffraction (SAED) and highresolution X-ray photoelectron spectroscopy (XPS). The size distributions of the nanoparticles were determined by transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) to an average diameter of (11 ± 6) to (38 ± 17) nm for the REF3-NPs from [BMIm][BF4]. The RE-NPs from [BMIm][NTf2] or PC showed diameters of (1.5 ± 0.5) to (5 ± 1) nm. The characterization was completed by energy-dispersive X-ray spectroscopy (EDX). © 2018 Siebels et al.