Thermolytic synthesis of cobalt and cobalt sulfide nanoparticles using Cobalt(II) N ^ O Schiff base complexes as single molecular precursors
Two novel N∧∧\wedge O-type Schiff base ligands and the corresponding Co(II)
complexes are reported. Thermogravimetric analysis indicated that the
complexes are potential molecular precursors for the fabrication of cobalt
and cobalt-containing nanomaterials. The significant difference in the
thermal decomposition profiles is recognized as an influence of structural
differences on the complexes. Thus, the complexes were thermally decomposed
using the melt and hot injection methods to examine the properties of the
obtained cobalt and cobalt sulfide nanoparticles, respectively. The reaction
parameters employed during the fabrication processes, in addition to
structural differences, influenced the morphological and crystallographic
phases and magnetic properties of the synthesized nanoparticles. We have
investigated the morphological properties and the crystallographic phase
compositions of the nanoparticles by various electron microscopy and
diffraction techniques, as well as energy-dispersive X-ray spectroscopy. The
melt reactions produced phase-pure cobalt nanoparticles, which exhibit
ferromagnetic behavior. The hot injection method utilized 1-dodecanethiol
(DDT) as both sulfur source and capping agent. We indexed the DDT-capped
cobalt sulfide nanoparticles to cubic Co99_{9}S88_{8} and Co33_{3}S44_{4}
phases using powder X-ray diffraction, high-resolution transmission electron
microscopy imaging, and selected area electron diffraction. The crystallite
sizes for Co99_{9}S88_{8} and Co33_{3}S44_{4} nanoparticles, based on the
Scherrer equation, were 12.4 nm and 14.1 nm, respectively. We find
significant differences in the magnetic properties, attributed to
nonmagnetic inclusions and vacancies due to the presence of S atoms.
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