The increasing presence of pharmaceutical pollutants, such as acetaminophen, in water bodies poses a significant environmental challenge due to their persistence and potential toxicity. This study investigated the enhanced photodegradation of acetaminophen using ZnO-NiO nanofibers as superior photocatalysts. The nanofibers synthesized with varying NiO contents (designated as ZN0.5, ZN1, ZN1.5, and ZN2), were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman, FTIR, Brunauer–Emmett–Teller (BET) analysis, and diffuse reflectance spectroscopy (DRS) to elucidate their structural, morphological, and optical properties. Thermogravimetric analysis (TGA) indicated that the nanofibers exhibit high thermal stability, with major weight loss attributed to the decomposition of the polymer matrix and residual organics. The BET analysis revealed that the specific surface area remains stable after increasing the NiO content up to a certain ratio. This stability correlates with the enhanced photocatalytic performance due to increased light absorption and improved charge separation. The diffuse reflectance spectra and Kubelka–Munk plots demonstrated a reduction in bandgap energy with higher NiO content, facilitating greater visible light absorption. Photocatalytic experiments under visible light irradiation, in the presence of peroxymonosulfate (PMS), showed that the ZN1.5 nanofibers achieved the highest acetaminophen degradation rate, i.e., 92%, within 3 h. Mechanistic studies, supported by radical trapping experiments, revealed that the improved photocatalytic efficiency is due to the synergistic effects of ZnO and NiO heterojunctions, which enhance charge separation and reactive oxygen species (ROS) generation. This research highlights the potential of ZnO-NiO nanofibers as effective photocatalysts for the degradation of pharmaceutical pollutants. The findings demonstrate that optimizing the composition and structure of nanofibers can significantly improve their environmental remediation capabilities, providing a promising solution for sustainable water treatment.

Molybdenum carbide co-catalyst and carbon nanofiber matrix are suggested to improve the nickel activity toward methanol electrooxidation process. The proposed electrocatalyst has been synthesized by calcination electrospun nanofiber mats composed of molybdenum chloride, nickel acetate, and poly (vinyl alcohol) under vacuum at elevated temperatures. The fabricated catalyst has been characterized using XRD, SEM, and TEM analysis. The electrochemical measurements demonstrated that the fabricated composite acquired specific activity for methanol electrooxidation when molybdenum content and calcination temperature were tuned. In terms of the current density, the highest performance is attributed to the nanofibers obtained from electrospun solution having 5% molybdenum precursor compared to nickel acetate as a current density of 107 mA/cm² was generated. The process operating parameters have been optimized and expressed mathematically using the Taguchi robust design method. Experimental design has been employed in investigating the key operating parameters of methanol electrooxidation reaction to obtain the highest oxidation current density peak. The main effective operating parameters of the methanol oxidation reaction are Mo content in the electrocatalyst, methanol concentration, and reaction temperature. Employing Taguchi’s robust design helped to capture the optimum conditions yielding the maximum current density. The calculations revealed that the optimum parameters are as follows: Mo content, 5 wt.%; methanol concentration, 2.65 M; and reaction temperature, 50 °C. A mathematical model has been statistically derived to describe the experimental data adequately with an R² value of 0. 979. The optimization process indicated that the maximum current density can be identified statistically at 5% Mo, 2.0 M methanol concentration, and 45 °C operating temperature.