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The aim of the study was the production of thin composite nanofibrous mats PAN/TiO2 nanoparticles using the electrospinning method from solution of PAN/TiO2/DMF. TiO2 nanoparticles were obtained using sol-gel method. To prepare sol mixture, organic alkoxides precursor of titanium isopropoxide and water solution were used. Calcination of TiO-gel and following milling were carried out to obtain nanoparticles of TiO2 rutile phase. In order to analyze the structure of the obtained particles, we used X-ray diffraction analysis (XRD) and energy dispersive spectrometer (EDS). Analysis of the morphology and chemical composition of the resulting composite nanofibers were carried out using a scanning electron microscope (SEM) with EDS. The analysis of the optical properties and the energy band structure prepared nanoparticles and thin composite nanofibrous mats were determined by spectral analysis of the absorbance as a function of the energy of radiation obtained using a UV–Vis spectrophotometer.