Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate.

作者: Kai Schütte , Juri Barthel , Manuel Endres , Marvin Siebels , Bernd M. Smarsly

DOI: 10.1002/OPEN.201600105

关键词: MetalScherrer equationPropylene carbonateTetrafluoroborateTrifluoromethanesulfonateMaterials scienceElectrochemistryIonic liquidNuclear chemistryHexafluorophosphateInorganic chemistry

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

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