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Octahedral CdS hollow microcages were synthesized on the basis of the ion interface reaction process by using CdMoO 4 crystals as in situ sacrificial templates. The products were characterized by X-ray powder diffraction, transmission electron microscopy, field-emission scanning electron microscopy, and a BrunauerEmmett-Teller plot. The results show that the shells of the obtained octahedral CdS microcage are constructed by nanoparticles or nanoplates with Na 2 S or thioacetamide as the sulfur source, respectively. The method using metal salts as the sacrificial template to prepare a hollow structure can be widely applied to synthesize other chalcogenides.