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A new type of environmental-friendly flexible nanofibers of aluminum doped zinc oxide (AZO) coated carbon (AZO@C) was successfully prepared by using polyvinyl alcohol (PVA) as raw materials. The as-spun PVA nanofibers were prepared <i>via</i> electrospinning and its water resistance was greatly improved after heat-treatment. Then, the PVA nanofibers with a layer of zinc aluminum hydroxide on the surface were synthesized by hydrothermal method. Thereafter, new AZO@C composite nanofibers was produced after sintering at 500℃ to the carbonization of PVA nanofibers and the dehydration of zinc aluminum hydroxide to form AZO nanoparticles. The structure and properties of the samples were characterized by Fourier-transform infrared spectrometer (FT-IR), thermal gravimetric analyzer (TGA) and scanning electron microscope (SEM). The average diameter of the AZO@C nanofibers is (320&#177;45)nm. The photocatalytic property of the resultant composite fibers is demonstrated by degrading methyl orange under solar light.