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A new class of nanocomposites based on organic and inorganic species integrated at a nanoscale has obtained more attention these years. Organic-inorganic hybrids have both the advantages of organic materials, such as light weight, flexibility and good moldability, and inorganic materials, such as high strength, heat stability and chemical resistance. In this work, PVAc/TiO2 organicinorganic hybrid was prepared by sol-gel process. Electrospinning technique was used to fabricate PVAc/TiO2hybrid nanofibers. The structures and properties of the hybrid nanofibers were characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscope (AFM),Differential Scanning Calorimeter (DSC) and Fouriertransform infrared (FTIR) spectra. SEM and AFM were employed to study the topography of the hybrid nanofibers.The chemical structure of the hybrid nanofibers were examined by FTIR. The DSC scansrevealed the second order transition temperature of the hybrid materials were higher than PVAc.