Lithiumpyridinyl-Driven Synthesis of High-Purity Zero-Valent Iron Nanoparticles and Their Use in Follow-Up Reactions

Alexander Egeberg, Theresa Block, Oliver Janka, Olivia Wenzel, Dagmar Gerthsen, Rainer Pöttgen, Claus Feldmann

8 Citations (Scopus)

Abstract

The synthesis of zero-valent iron (Fe(0)) nanoparticles in pyridine using lithium bipyridinyl ([LiBipy]) or lithium pyridinyl ([LiPy]) is presented. FeCl3 is used as the most simple starting material and reduced either in a [LiBipy]-driven two-step approach or in a [LiPy]-driven one-pot synthesis. High-quality nanoparticles are obtained with uniform, spherical shape, and mean diameters of 2.9 ± 0.5 nm ([LiBipy]) or 4.1 ± 0.7 nm ([LiPy]). The as-prepared, high purity Fe(0) nanoparticles are monocrystalline. In addition to particle characterization (high-resolution transmission electron microscopy, scanning transmission electron microscopy, dynamic light scattering), composition and purity are examined in detail based on electron diffraction, X-ray powder diffraction, elemental analysis, infrared spectroscopy, 57 Fe Mössbauer spectroscopy, and magnetic measurements. Due to their small size and high purity, the Fe(0) nanoparticles are highly reactive. They can be used in follow-up reactions to obtain a variety of iron compounds, which is exemplarily shown for the transformation to iron carbide (Fe3 C) nanoparticles, the reaction with sulfur to obtain FeS nanoparticles, or the direct reaction with pentamethylcyclopentadiene to FeCp*2 (Cp*: pentamethylcyclopentadienyl).

Original languageEnglish
Article number1902321
JournalSmall (Weinheim an der Bergstrasse, Germany)
Volume15
Issue number37
Pages (from-to)e1902321
ISSN1613-6810
DOIs
Publication statusPublished - 1 Sept 2019
Externally publishedYes

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