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Lithiumpyridinyl‐Driven Synthesis of High‐Purity Zero‐Valent Iron Nanoparticles and Their Use in Follow‐Up Reactions
Author(s) -
Egeberg Alexander,
Block Theresa,
Janka Oliver,
Wenzel Olivia,
Gerthsen Dagmar,
Pöttgen Rainer,
Feldmann Claus
Publication year - 2019
Publication title -
small
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 3.785
H-Index - 236
eISSN - 1613-6829
pISSN - 1613-6810
DOI - 10.1002/smll.201902321
Subject(s) - nanoparticle , materials science , transmission electron microscopy , lithium (medication) , dynamic light scattering , mössbauer spectroscopy , particle size , scanning electron microscope , scanning transmission electron microscopy , high resolution transmission electron microscopy , chemical engineering , analytical chemistry (journal) , nuclear chemistry , crystallography , nanotechnology , chemistry , organic chemistry , medicine , endocrinology , engineering , composite material
The synthesis of zero‐valent iron (Fe(0)) nanoparticles in pyridine using lithium bipyridinyl ([LiBipy]) or lithium pyridinyl ([LiPy]) is presented. FeCl 3 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 (Fe 3 C) nanoparticles, the reaction with sulfur to obtain FeS nanoparticles, or the direct reaction with pentamethylcyclopentadiene to FeCp* 2 (Cp*: pentamethylcyclopentadienyl).