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This research investigates the influence of synthesis kinetics on the structural and photocatalytic properties of chitosan–clay nanocomposites (Cs/MMT) and chitosan–hectorite nanocomposites (Cs/HET), employing an optimized initial stoichiometry of 1:3. Utilizing a variety of analytical techniques, including X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FTIR), the study explores the structural evolution of the nanocomposites and their photocatalytic performance using semiconductor catalysts TiO₂ and ZnO. The findings emphasize the significant impact of reaction kinetics, particularly after 3 h of reaction time, on the structural features of the nanocomposites. Notably, Cs/MMT demonstrates greater crystalline stability compared to Cs/HET due to variations in octahedral cavity occupancy in the initial clays. FTIR and TEM analyses depict the progressive evolution of the nanocomposites during the reaction, shedding light on how reaction kinetics drive the formation of specific bonds within the nanocomposites. In terms of photocatalytic activity, this study provides insights into the complex dynamics of photocatalytic degradation, with a specific focus on the performance of TiO₂ and ZnO under diverse experimental conditions. The superior efficacy of TiO₂ as a catalyst, particularly when integrated with Cs/MMT nanocomposites, is unequivocally demonstrated, with degradation rates exceeding 80%. This preference stems from TiO₂ consistently exhibiting higher degradation rates compared to ZnO, attributed to structural disparities between montmorillonite and hectorite, influencing catalyst–support interactions. The findings underscore the critical importance of selecting suitable catalyst and support matrix combinations for optimizing performance in specific applications. Full article

The photocatalytic degradation process and absorption kinetics of the aqueous solution of the Cibacron Brilliant Yellow 3G-P dye (Y) were investigated under UV-Vis light. Pure barium titanate BaTiO₃ (BT) and cobalt ion-substituted barium Ba_1−xCo_xTiO₃ (x = 0, …, 1) nano-compound powders (BCT) were synthesized using the sol–gel method and colloidal solution destabilization, and utilized as photocatalysts. The powder X-ray diffraction (PXRD) crystal structure analysis of the BT nanoparticles (NPs) revealed a prominent reflection corresponding to the perovskite structure. However, impurities and secondary phase distributions were qualitatively identified in the PXRD patterns for x ≥ 0.2 of cobalt substitution rate. Rietveld refinements of the PXRD data showed that the BCT nano-compound series undergoes a transition from perovskite structure to isomorphous ilmenite-type rhombohedral CoTiO₃ (CT) ceramic. The nanoparticles produced displayed robust chemical interactions, according to a Fourier transform infrared spectroscopy (FTIR) analysis. The BT and BCT nanoparticles had secondary hexagonal phases that matched the PXRD results and small aggregated, more spherically shaped particles with sizes ranging from 30 to 114 nm, according to transmission electron microscopy (TEM). Following a thorough evaluation of BCT nano-compounds with (x = 0.6), energy-dispersive X-ray (EDX) compositional elemental analysis revealed random distributions of cobalt ions. Through optical analysis of the photoluminescence spectra (PL), the electronic structure, charge carriers, defects, and energy transfer mechanisms of the compounds were examined. Due to the cobalt ions being present in the BT lattice, the UV-visible absorption spectra of BCT showed a little red-shift in the absorption curves when compared to pure BT samples. The electrical and optical characteristics of materials, such as their photon absorption coefficient, can be gathered from their UV-visible spectra. The photocatalytic reaction is brought about by the electron–hole pairs produced by this absorption. The estimated band gap energies of the examined compounds, which are in the range of 3.79 to 2.89 eV, are intriguing and require more investigation into their potential as UV photocatalysts. These nano-ceramics might be able to handle issues with pollution and impurities, such as the breakdown of organic contaminants and the production of hydrogen from water. Full article