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Yes / In this study, we prepared chitosan (Cs_P) nanofibers (NFs) membrane by electrospinning. The Cs_P NFs membrane was then chemically functionalized (CsF) by a novel stepwise chemical process. The CsF NFs membrane was electrospray with TiO2 nanoparticles (NPs) to prepare the CsF_Coa NFs membrane. A second NFs membrane with embedded TiO2 NPs (Cs_Co) was also prepared by electrospinning. The TiO2 NPs, Cs_P, CsF s, CsF_Coa NFs, and Cs_Co NFs membranes were analyzed by standard spectroscopic, microscopic, X-ray, and thermal methods. Fourier transform infrared (FTIR) analysis confirmed the incorporation of the new functional group into the Cs structure. X-ray photoelectron spectroscopy (XPS) data confirmed the FTIR results and the fabrication of the CsF NFs membrane. Scanning electron microscope (SEM) micrographs showed a smooth morphology for the Cs_P NFs membrane and a denser morphology for the CsF NFs membrane (NFs swelled with functionalization). The SEM micrographs also showed a dense cloud of TiO2 NPs on the surface of the Cs_Coa NFs membrane. Transmission electron microscope (TEM) showed that the particle size of TiO2 NPs varied between 20 and 35 nm and tended to be spherical. The X-ray diffraction (XRD) pattern confirmed the existence of the anatase phase of the TiO2 NPs. The presence of TiO2 in the Cs_Coa and Cs_Co NFs membranes was also confirmed by energy-dispersive x-ray spectroscopy (EDX). Surface profilometry confirmed an increase in the surface roughness of the CsF and Cs_Coa NFs membranes. Brunauer–Emmett–Teller (BET) analysis revealed that the isotherms and hystereses for all NFs membranes were of the IV and H3 types, respectively, corresponding to mesopores and slit pores. The higher photocatalytic activity of the Cs_Coa NFs membrane (89%) compared to the Cs_Co NFs membrane (40%) was attributed to a balance between the short band gap, high surface roughness, and lower surface area.