Titania (TiO2)/PVP composite nanofibers were prepared with electrospinning method followed by calcining in air at different temperatures. The nanofibers were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectrum and photoluminescence (PL) spectrum. The results showed that the nanofibers are uniform and have an average diameter of similar to 40 nm. It is also found that the photoluminescence properties were largely influenced by different crystalline structure. The nanofibers yield visible photoluminescence peaking at 550 nm for anatase phase and near infrared photoluminescence peaking at 820 nm for rutile phase. (c) 2007 Published by Elsevier B.V.