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In this work, TiO2 nanoparticles were successfully synthesized with narrow size distribution via a wet ball milling sol-gel method. The effect of calcination temperature on photocatalytic activity was observed from particle size, crystallite size, and phase transition of TiO2 nanoparticles. Increasing calcination temperature increased particle size, crystallite size, and the crystallinity of synthesized TiO2. Phase transition depended on variation in calcination temperatures. A two-phase mixture of anatase and brookite was obtained with lower calcination temperature whereas a three-phase mixture appeared when calcination temperature was 500–600 °C. With higher temperature, the rutile phase kept increasing until it was the only phase observed at 800 °C. Anatase strongly affected the photocatalytic activity from 300 °C to 600 °C while the particle size of TiO2 was found to have a dominant effect on the photocatalytic activity between 600 °C and 700 °C. A mixture of three phases of TiO2-600 exhibited the highest methylene blue degradation with the rate constant of 9.46 × 10−2 h−1 under ultraviolet (UV) irradiation.

Effect of Calcination Temperature on Photocatalytic Activity of Synthesized TiO2 Nanoparticles via Wet Ball Milling Sol-Gel Method