Nickel titanate/poly(vinyl acetate) (PVAc) composite nanofibers were prepared by sol-gel processing and electrospinning technique. Rhombohedral nickel titanate fibers with 150-200nm diameter were obtained by high temperature calcination of the composite fibres. Structural, morphological and crystalline phase features of electrospun NiTiO3 fibers were studied by SEM, AFM, XRD and FT-IR. The fibrous nature of nickel tiatanate was stable even after calcination at 1273 K. (C) 2004 Elsevier B.V. All rights reserved.