• • Mesopore size of 4.4 nm achieved a gemcitabine loading of 228 mg g−1, a 3.7-fold increase in combined therapy cytotoxicity over monotherapy, and >70% drug release under NIR irradiation, demonstrating the critical balance between pore architecture and therapeutic payload.
• • Photothermal conversion efficiency reached 62% via N-doping and defect engineering, enabling NIR-triggered hyperthermia that enhances tumor permeability and drug release kinetics.
• • Biocompatibility exceeded 95% cell viability at 200 μg mL−1, while combined therapy reduced tumor cell viability to ~5% at 25 μg mL−1, indicating a wide therapeutic window and potent antitumor efficacy.
• • Pore size control via kinetic modulation of resin polymerization and TEOS hydrolysis allows scalable synthesis of mC with tunable mesopores (2-5 nm), directly linking structural parameters to functional performance in photothermal-chemotherapy.