Journalartikel

Jahr der Veröffentlichung: 2017

Seiten: 137-148

Zeitschrift: ChemistryOpen

Bandnummer: 6

Heftnummer: 1

ISSN: 2191-1363

DOI Link: https://doi.org/10.1002/open.20160010

Verlag: Wiley

Abstract: 
Decomposition of transition-metal amidinates [M{MeC(N/Pr)(2)}(n)] [M(AMD) n; M= Mn", Fe", Co", Ni", n= 2; Cu', n= 1) induced by microwave heating in the ionic liquids (ILs) 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]), 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIm][PF6]), 1-butyl-3methylimidazolium trifluoromethanesulfonate (triflate) ([BMIm] [TfO]), and 1-butyl-3-methylimidazolium tosylate ([BMIm][Tos]) or in propylene carbonate (PC) gives transition-metal nanoparticles (M-NPs) in non-fluorous media (e.g. [BMIm][Tos] and PC) or metal fluoride nanoparticles (MF2-NPs) for M= Mn, Fe, and Co in [BMIm][BF4]. FeF2-NPs can be prepared upon Fe(AMD)(2) decomposition in [BMIm][BF4], [BMIm][PF6], and [BMIm][TfO]. The nanoparticles are stable in the absence of capping ligands (surfactants) for more than 6 weeks. The crystalline phases of the metal or metal fluoride synthesized in [BMIm][BF4] were identified by powder X-ray diffraction (PXRD) to exclusively Ni-and Cu-NPs or to solely MF2-NPs for M= Mn, Fe, and Co. The size and size dispersion of the nanoparticles were determined by transmission electron microscopy (TEM) to an average diameter of 2(+/- 2) to 14(+/- 4) nm for the M-NPs, except for the Cu-NPs in PC, which were 51(+/- 8) nm. The MF2-NPs from [BMIm][BF4] were 15(+/- 4) to 65(+/- 18) nm. The average diameter from TEM is in fair agreement with the size evaluated from PXRD with the Scherrer equation. The characterization was complemented by energy-dispersive X-ray spectroscopy (EDX). Electrochemical investigations of the CoF2-NPs as cathode materials for lithium-ion batteries were simply evaluated by galvanostatic charge/discharge profiles, and the results indicated that the reversible capacity of the CoF2-NPs was much lower than the theoretical value, which may have originated from the complex conversion reaction mechanism and residue on the surface of the nanoparticles.

Harvard-Zitierstil: Schütte, K., Barthel, J., Endres, M., Siebels, M., Smarsly, B., Yue, J., et al. (2017) Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate, ChemistryOpen, 6(1), pp. 137-148. https://doi.org/10.1002/open.20160010

APA-Zitierstil: Schütte, K., Barthel, J., Endres, M., Siebels, M., Smarsly, B., Yue, J., & Janiak, C. (2017). Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate. ChemistryOpen. 6(1), 137-148. https://doi.org/10.1002/open.20160010