Nickel-doped zinc oxide (NiZ) nanofibres (NFs) were fabricated using sol-gel electrospinning (ES) technique followed by pyrolysis from an aqueous solution of polyvinyl alcohol/zinc acetate/nickel acetate tetrahydrate. The morphology of the NiZ NFs was analyzed using Scanning Electron Microscopy (SEM), which revealed a uniform and well-defined fibrous structure. X-ray diffraction (XRD) results indicated complete removal of the organic phase from NiZ NFs during pyrolysis. The structural analysis confirmed the incorporation of Nickel (Ni) into the Zinc oxide (ZnO) lattice without altering its wurtzite crystal structure. The optical properties and bandgap variations were evaluated using UV-visible spectroscopy, which indicated a bandgap narrowing with increasing Nickel doping. The Photoluminescence (PL) spectroscopy confirmed the presence of defect states and recombination processes in the NFs. The gas sensing performance was investigated by measuring the response to various analytes at a concentration of 50 ppm with varying operating temperatures. The results indicated that the highest response was observed for 5 w% NiZ NFs towards acetone vapors. The response and recovery time were recorded at 80 seconds and 60 seconds. The enhanced sensitivity is attributed to the optimal doping concentration, which significantly improves the surface reaction and charge carrier mobility.
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