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Electrospinning processes have several attractive advantages such as comparatively low cost,applicability to various materials,and the ability to generate relatively large-scale continuous films.Many inorganic micro/nanofibers have been fabricated using electrospinning techniques [1].Hydrothermal methods also give a uniform composition,pure products,monodispersed particles,and control of the shape and size of the particles [2].In this work,titanium isopropoxide/poly(methyl methacrylate) (TIP/PMMA) fibers were successfully prepared using sol–gel and electrospinning techniques.Crystalline TiO2 nanofibers were obtained using a hydrothermal reaction or calcinations treatment.The effects of the production method on the crystal structures were examined,and the TiO2 nanofibers used to photocatalyst for decomposition of methylene blue.The TiO2 nanofibers prepared by hydrothermal reaction than calcinations treatment could be obtained to anatase phase of the small crystallite size.These photocatalysts were evaluated based on the photodecomposition of methylene blue under ultraviolet light.The kinetic constant (k1) of the hydrothermal-185,calcination-450,and calcination-500 samples were 7.40 × 10-3,2.21 × 10-2,and 1.55 ×10-2,respectively.The TiO2 nanofibers prepared using calcination had higher efficiencies than those prepared using a hydrothermal reaction,but the TiO2 nanofibers prepared without calcination could be used as photocatalysts.