Size-controlled In2O3 hollow structures have been successfully prepared by a two-step process. Indium(III)–benzenedicarboxylate (In–BDC) hexagonal rods with different sizes were first obtained on a large scale via a simple solution reaction using indium(III) nitrate and 1,4-benzenedicarboxylic acid as starting reactants and DMF as solvent with addition of sodium acetate. Then In2O3 hollow structures were prepared by annealing In–BDC complexes. It was found that the concentration of sodium acetate is important in determining the size of In–BDC hexagonal rods as well as the formation of In2O3 hollow structures. The products were characterized by X-ray diffraction (XRD), energy dispersive spectrometry (EDS), selected area electron diffraction (SAED), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution TEM (HRTEM). In addition, In2O3 hollow structures were further studied by Raman and room-temperature photoluminescence.
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