In this paper, we have systematically studied the structural, morphological, and optical properties of Ni-doped TiO2, synthesized via a simple, cost-effective electrospinning method followed by calcination at 500 °C. The nanofibers with a core-shell structure were relatively homogeneous, smooth and randomly oriented, and there were no significant differences in fiber diameters due to Ni2+ content. Core loss mapping using electron energy loss spectroscopy confirmed an even distribution of titanium and relatively uniform nickel in the fibers. It was found that doping with 0.5 mol.% Ni2+ decreased the rutile content, while doping with 1 mol.% Ni2+resulted in a pure anatase phase with a significantly increased specific surface area (36.6 m2/g). Further increase in Ni2+ content (3–10 mol.%) not only prolonged the response of TiO2 nanofibers to visible light, but also increased the specific surface area (49.5 m2/g), decreased crystallite size (7 nm), and increased rutile content in TiO2 (33 wt.%). Photoluminescence analysis revealed that doping TiO2 with different amounts of Ni2+ leads to a gradual decrease of emission spectra intensity and red shift in the maxima positions. The XPS results confirmed that as the Ni2+ content enlarged, the Ti2+ and Ti3+ content increased significantly, effectively promoting the formation of oxygen vacancies. Raman analysis showed that an increase in nickel content (3–5 mol.%) led to a decrease and shift in peak intensity due to Ti3+ formation and also the possible presence of NiTiO3 phases. HRTEM analysis showed that Ni was doped into the substitution sites of both the anatase and rutile TiO2 lattice but had a stronger influence on the distortion of the anatase phase. The photocatalytic activity of Ni-doped TiO2 nanofibers was explored by analyzing the degradation of an antibiotic, oxytetracycline, monitored in laboratory conditions under visible light irradiation. After 60 min of irradiation, the degradation of OTC with 1Ni-TiO2 reached 76.4 % and with 10Ni-TiO2 70.5 %.
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