In this paper, weak acids, weak bases or their mixtures were used as reaction media/coordinating ligands to achieve systematic morphological control over amphoteric indium oxide nanostructures. Different indium/oleic acid molar ratios from 1 : 0, 1 : 1, 1 : 2, 1 : 3, 1 : 6 and 1 : 15 in non-coordinating, weakly coordinating, strongly coordinating and their mixed media were adopted to prepare irregular aggregated nanoparticles and uniform regular/truncated octahedra, etc. In addition to their strong size-dependent absorption, single-crystalline indium oxide octahedra also gave a strong band-edge emission while irregular indium oxide aggregated nanoparticles only exhibited a weak deep-trap emission. Meanwhile, the truncated octahedra were self-assembled into either zigzag lines or pentagram patterns, and the regular octahedra and truncated cubes were self-assembled into hexagonally packed nanocrystal arrays. In addition, the formation mechanism of the various nanostructures under different conditions was investigated in detail.
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