A novel method using Cu(AC) 2 ·H 2 O and dimethylglyoxime as reagents has been successfully developed for the controllable synthesis of Cu 2 O microcrystals with distinctive morphologies, including porous hollow microspheres, octahedral microcages, and microcrystals with truncated corners and edges and octahedral microcrystals. These structures can be fine-tuned by varying reaction temperature, reaction time, and concentration. The products were characterized by Xray diffraction, field emission scanning electron microscopy, X-ray photoelectron spectra, and UV/Vis diffuse reflectance spectra. This is the first report of the preparation of the novel microcage structure of Cu 2 O through a simple solution-based route. By investigating the intermediate products which resemble the final crystal structures, a possible growth mecha-
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