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Mechanochemically Synthesized Nanocrystalline Sb_2S_3 Particles

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Nanocrystalline Sb_2S_3 particles have been synthesized from Sb and S powders by high-energy milling in a planetary mill using argon protective atmosphere. X-ray diffraction, particle size analysis, scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, electron diffraction, high resolution transmission electron microscopy, UV-VIS, and differential scanning calorimetry methods for characterization of the prepared particles were applied. The powder X-ray diffraction pattern shows that Sb_2S_3 nanocrystals belong to the orthorhombic phase with calculated crystallite size of about 36 nm. The nanocrystalline Sb_2S_3 particles are constituted by randomly distributed crystalline nanodomains (20 nm) and then these particles are forming aggregates. The monomodal distribution of Sb_2S_3 particles with the average hydrodynamic parameter 210 nm was obtained. The quantification of energy dispersive X-ray spectroscopy analysis peaks give an atomic ratio of 2:3 for Sb:S. The optical band gap determined from the absorption spectrum is 4.9 eV, indicating a considerable blue shift relative to the bulk Sb_2S_3. Differential scanning calorimetry curves exhibit a broad exothermic peak between 200 and 300°C, suggesting recovery processes. This interpretation is supported by X-ray diffraction measurements that indicate a 23-fold increase of the crystallite size to about 827 nm as a consequence of application of high temperature process. The controlled mechanochemical synthesis of Sb_2S_3 nanoparticles at ambient temperature and atmospheric pressure remains a great challenge.
Physical description
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