In this work, Zn2+-doped TiO2:WO3 nanostructured films, with different doping levels, were produced by electrospinning followed by sintering, and tested as potential materials for relative humidity (RH) detection. The best results are directly related to the microstructure, lower bandgap and aggregation of metal oxide nanocomposite in the electrospun membrane, compared to the support-free MON. In addition, the highest photodegradation efficiency was noted for the systems with 5 wt% vanadium oxide dispersed in the fibers (92% dye degradation in 120 min of exposure to the light source), with recyclability of the composite material for use in new photocatalysis cycles. The fiber-supported MON showed photoactivity for rhodamine B dye degradation using visible light. The reflectance spectra showed that the bandgap of the MON was progressively decreased (3.20 to 2.11 eV) with the V5+ ions doping level increase. Microstructural characterization of the samples was performed by XRD, SEM, EDS, Raman, and DSC techniques. In this work, 5+-doped nanostructures were prepared by the sintering process at 500 ☌ and supported in electrospun fiber membranes for application as photocatalyst devices. In addition, the use of polymer membrane-supported MON is preferable to prevent further aggregation of particles, increase the surface area of the semiconductor in contact with the contaminant, and enable material reuse without considerable efficiency loss. These superior properties have been observed for TiO2 - based MON, which exhibit improved structural stability and photoactivity in environmental decontamination processes. Metal oxide nanocomposites (MON) have gained significant attention in the literature for the possibility of improving the optical and electronic properties of the hybrid material, compared to its pristine constituent oxides. Additionally, the behavior of sample was studied as a function of temperature. The value of crystal size determined from X-ray data was in good agreement with that informed by the supplier. The average absolute divergence does not exceed 0.70 nm. To establish a relation between the result obtained with modified Scherrer's equation and the nominal average crystal size, a statistical treatment and a comparative assessment were performed. From X-ray diffraction data, an average crystal size about 20.63 nm was achieved for unheated sample. The manufactured titanium dioxide-nanostructured powder with nominal average size about 21nm was used as the reference standard to determine the accurate of modified equation. In order to shed light about the nanomaterials sizing, a modified Scherrer's equation was applied to estimate more accurately the nanostructured titanium dioxide crystal size. The materials sizing in nano-scale is a challenge to be overcome, because the size determined by various methods differ.
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