Journal Article

FZJ-2017-07737

http://join2-wiki.gsi.de/foswiki/pub/Main/Artwork/join2_logo100x88.png Synthesis of Metal Nanoparticles and Metal Fluoride Nanoparticles from Metal Amidinate Precursors in 1-Butyl-3-Methylimidazolium Ionic Liquids and Propylene Carbonate

Schütte, K. ; Barthel, J.FZJ* ; Endres, M. ; Siebels, M. ; Smarsly, B. M. ; Yue, J. ; Janiak, C. (Corresponding author)

2017
Wiley-VCH-Verl. Weinheim

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Please use a persistent id in citations: http://hdl.handle.net/2128/15964  doi:10.1002/open.201600105

Abstract: Decomposition of transition-metal amidinates [M{MeC(NiPr)2}n] [M(AMD)n; 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]), 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIm][PF6]), 1-butyl-3-methylimidazolium 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.

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Contributing Institute(s):

1. Materialwissenschaft u. Werkstofftechnik (ER-C-2)

Research Program(s):

1. 143 - Controlling Configuration-Based Phenomena (POF3-143) (POF3-143)

Appears in the scientific report 2017

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Database coverage:
; ; ; ; Current Contents - Physical, Chemical and Earth Sciences ; DOAJ Seal ; IF < 5 ; JCR ; NCBI Molecular Biology Database ; SCOPUS ; Science Citation Index Expanded ; Thomson Reuters Master Journal List ; Web of Science Core Collection

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