AbstractAlveolate amorphous Sb2S3 microspheres about 2 μm in diameter were hydrothermally synthesized in aqueous solution without the use of a surfactant at 180 °C by using SbCl3, L‐cysteine, and tartaric acid as starting materials. After annealing at 250 °C for 3 h under a nitrogen atmosphere, polycrystalline Sb2S3 hollow spheres were obtained. The morphology, structure, and phase composition of alveolate Sb2S3 microspheres were characterized by X‐ray diffraction, field‐emission scanning electron microscopy, energy dispersive X‐ray analysis, and X‐ray photoelectron spectroscopy. It was demonstrated that tartaric acid and L‐cysteine play a key role in the formation of such hierarchical structures. In addition, the possible aggregation mechanism was proposed to illustrate the formation of Sb2S3 microspheres on the basis of the experimental results and analyses.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)
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