Mechanochemically synthesized nanocrystalline Sb2S3 particles.

摘要

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 diraction, particle size analysis, scanning electron microscopy, energy dispersive X-ray spectroscopy, transmission electron microscopy, electron diraction, high resolution transmission electron microscopy, UV-VIS, and dierential scanning calorimetry methods for characterization of the prepared particles were applied. The powder X-ray diraction 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 quantication 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. Dierential scanning calorimetry curves exhibit a broad exothermic peak between 200 and 300 C, suggesting recovery processes. This interpretation is supported by X-ray diraction 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.