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Decahedral TiO₂ decorated with bimetallic nanoparticles were synthesized via radiolysis and photodeposition method. The effect of bimetallic surface composition (Ag_Pt, Ag_Au, Au_Pd, Au_Pt) as well as deposition technique (simultaneous or sequential) on the photocatalytic activity in phenol degradation and efficiency of hydroxyl radicals generation under UV–vis light irradiation were investigated. Modified and pristine decahedral TiO₂ anatase with exposed {001} were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), transmission electron microscopy (TEM) with energy-dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), inductively coupled plasma-mass spectrometry (ICP-MS) and X-ray photoelectron spectroscopy (XPS). The gas chromatography-mass spectrometry was employed to detect organic intermediates to establish degradation pathway of …