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Abstract: Quasi-aligned, high-aspect-ratio AlN micro- and nanostructures were synthesized under high nitrogen pressure by the exothermic reaction of an Al+0.015mol (C2F4) n mixture. Structurally uniform AlN micro- and nanofibers with hexagonal and cylindrical morphologies were obtained when the system temperature was maintained within the range of 1600–1700°C. The fibers had aspect ratios as high as 2000, diameters in the range of ∼0.05–20μm, and were ∼100–1000μm in length. High-resolution transmission electron microscopic and selected area diffraction analyses indicated that the as-synthesized AlN micro- and nanostructures are perfectly single crystalline with preferential growth along the [001] direction. Branching was also observed in some of the micro-fibers, giving rise to randomized, two-dimensional comb textures. Based on the results obtained in the present study, a mechanism for the formation of AlN micro- and nanostructures under combustion conditions was proposed. [Copyright &y& Elsevier]