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SiC–Al2O3 hetero-structural nanofibers have been synthesized by the chemical solution approach at 200 ° C. The diameters of nanofibers are in the range of 60–100 nm while the lengths are from tens of micrometers to hundreds of micrometers. The microstructural analysis shows that the fibers possess a like-epitaxial relationship between (104) of hexagonal Al2O3 and (111) of cubic SiC. Additionally, the optical investigation of the nanofibers suggests there are some defects in the low annealing temperature synthesized SiC–Al2O3 nanofibers. [ABSTRACT FROM AUTHOR]