Article,

An Easy One-Pot Solvothermal Synthesis of Poorly Crystalline Solid Res2/C Microspheres

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Materials Chemistry and Physics, (2015)
DOI: 10.1016/j.matchemphys.2014.12.012

Abstract

Dense microspheres consisting of poorly crystalline ReS2 embedded in carbon were synthesized with a high yield via a facile one-pot solvothermal route, by reacting dirhenium decacarbonyl, elemental sulfur and an aromatic solvent (benzene, toluene or p-xylene) for 24 h at 180 degrees C. X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDS), Raman spectroscopy, and Fourier transform infrared spectroscopy (Fr-IR) techniques were used to characterize the samples. The resulting microspheres were dense, with average diameters between 0.79 and 1.40 mu m, had smooth surfaces and were constructed of ReS2 sheet-like structures with 4.5-9.8 wt % of structural amorphous carbon, which is retained as a textural stabilizer after calcination at 800 degrees C. The synthesis was repeated using isopropanol and cyclohexane, whose products were agglomerated grains and botryoidal quasi-spherical particles, respectively. A possible formation mechanism of ReS2/C microspheres was preliminarily presented, in order to clarify the mechanistic differences between the rhenium carbonyl and other transition metal carbonyls used in similar syntheses.

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