The synthesis of WS2 onion-like nanoparticles by means of a high-temperature metal–organic chemical vapor deposition (MOCVD) process starting from W(CO)6 and elemental sulfur is reported. The reaction can be carried out as a single-step reaction or in a two-step process where the intermediate products, amorphous WS2 nanoparticles, formed through the high-temperature reaction of tungsten and sulfur in the initial phase of the reaction, are isolated and converted into onion-type WS2 nanoparticles in a separate annealing step. Analysis of the reaction product using X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) combined with energy dispersive X-ray spectroscopy (EDX) allowed to optimize the reaction in such a way that filled onion-like structures are formed in a one-step reaction, whereas hollow onion-like structures are obtained by the two-step procedure. A model could be devised that allows us to rationalize the different outcome of the reactions. The MOCVD approach therefore allows a selective synthesis of open and filled fullerene-like chalcogenide nanoparticles.
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