1：Experimental Design and Method Selection:

The study used spray pyrolysis for synthesizing TiO2 microspheres, followed by post-modification via calcination to enhance photocatalytic properties. Characterization methods included XRD, SEM, and N2 adsorption to analyze structure and surface area. Photocatalytic activity was assessed through methylene blue degradation under UV light.

2：Sample Selection and Data Sources:

TiO2 sol was prepared from titanium (IV) isopropoxide in isopropyl alcohol with DI water. Samples were synthesized at pyrolysis temperatures of 500, 600, and 700°C, and post-modified by calcination at various temperatures.

3：List of Experimental Equipment and Materials:

Equipment included ultrasonic vibrators (1.7 MHz), furnaces with PID controller, thimble filter, heating tape, N2 porosimeter (Tristar 3020, Micromeritics), XRD (Miniflex 600, Rigaku), HR FE-SEM (MERLIN, Carl Zeiss), UV-visible spectrophotometer (Optizen POP, Mecasys), and a 400 W mercury lamp. Materials included TTIP (97% Aldrich), isopropyl alcohol (99.7%, Carlo), DI water, nitric acid, and methylene blue dye.

4：7 MHz), furnaces with PID controller, thimble filter, heating tape, N2 porosimeter (Tristar 3020, Micromeritics), XRD (Miniflex 600, Rigaku), HR FE-SEM (MERLIN, Carl Zeiss), UV-visible spectrophotometer (Optizen POP, Mecasys), and a 400 W mercury lamp. Materials included TTIP (97% Aldrich), isopropyl alcohol (7%, Carlo), DI water, nitric acid, and methylene blue dye. Experimental Procedures and Operational Workflow:

4. Experimental Procedures and Operational Workflow: TiO2 sol was prepared by hydrolysis and condensation, nebulized with ultrasonic vibrators, and pyrolyzed at set temperatures. Particles were collected, characterized, and tested for photocatalytic activity by degrading MB under UV light with stirring and temperature control.

5：Data Analysis Methods:

Data from characterization tools were used to determine crystallinity, morphology, surface area, and pore size. Photocatalytic efficiency was measured by monitoring MB concentration over time using UV-visible spectrophotometry.