Mechanochemically Synthesized Nanocrystalline Sb2S3 Particles |
| E. Dutkováa, M.J. Sayagués b, C. Real b, A. Zorkovská a, P. Baláž a, A. Šatka c, J. Kováč c and J. Ficeriová a
aInstitute of Geotechnics, Slovak Academy of Sciences, Watsonova 45, 04001 Košice, Slovakia bInstitute of Material Sciences of Seville (CSIC-US), Spain cInstitute of Electronics and Photonics, Slovak University of Technology, Bratislava, Slovakia |
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| Nanocrystalline Sb2S3 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 Sb2S3 nanocrystals belong to the orthorhombic phase with calculated crystallite size of about 36 nm. The nanocrystalline Sb2S3 particles are constituted by randomly distributed crystalline nanodomains (20 nm) and then these particles are forming aggregates. The monomodal distribution of Sb2S3 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 Sb2S3. 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 Sb2S3 nanoparticles at ambient temperature and atmospheric pressure remains a great challenge. |
DOI: 10.12693/APhysPolA.126.943 PACS numbers: 81.05.Hd, 81.07.Bc, 81.20.Wk |