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This study investigated the synthesis of two different types of photocatalysts, namely, boron/sodium fluoride co-doped titanium dioxide (B/NaF-TiO₂), and its analogue, a dye-sensitized form of silicon-based axial methoxy substituted phthalocyanine (B/NaF-TiO₂SiPc). Structural and morphological characterizations were performed via X-ray diffraction (XRD); Fourier transform infra-red (FTIR); N₂ adsorption–desorption at 77 K by Brunauer–Emmett–Teller (BET) and Barrett, Joyner, and Halenda (BJH) methods; transmission electron microscopy (TEM); X-ray photoelectron spectroscopy (XPS); and UV–visible absorption spectroscopy. The estimated crystallite size of pure TiO₂ and pure B/NaF-TiO₂ was 24 nm, and that of B/NaF-TiO₂SiPc was 29 nm, whereas particle sizes determined by TEM were 25, 28, and 31 nm for pure TiO₂, B/NaF-TiO₂ and B/NaF-TiO₂SiPc respectively. No significant differences between B/NaF-TiO₂ and B/NaF-TiO₂SiPc were observed for surface area by (BET) analysis (13 m²/g) or total pore volume by the BJH application model (0.05 cm³/g). Energy band gap values obtained for B/NaF-TiO₂ and B/NaF-TiO₂SiPc were 3.10 and 2.90 eV respectively, lower than pure TiO₂ (3.17 eV). The photocatalytic activity of the synthesized materials was tested using carbamazepine (CBZ) as the model substrate. Carbamazepine removal after 4 h of irradiation was almost 100% for B/NaF-TiO₂ and 70% for B/NaF-TiO₂SiPc; however, the substrate mineralization proceeded slower, suggesting the presence of organic intermediates after the complete disappearance of the pollutant.