This study pioneers novel boron-based materials with transformative potential for boron neutron capture therapy (BNCT). We initiate by synthesizing highly water-dispersible boron nitride (10BN) nanoparticles through solvothermal techniques, unveiling distinctive structural features. 10BN-treated HeLa cells exhibit noteworthy anti-tumor efficacy, resulting in ~50% cell mortality. Concurrently, boron carbide quantum dots (B4C QDs) are fabricated, showcasing elevated fluorescence in tumor cells due to inherent defect states. Cytotoxicity assessments and BNCT evaluations position B4C QDs as compelling alternatives to conventional boron agents. Moreover, our exploration extends to boron carbon nitride (BCN), produced via solvothermal means, unveiling a hexagonal structure enriched with defect states and porous layered arrangement. BCN manifests potent anti-tumor effects surpassing BN, B4C, and clinically studied L-BPA on HeLa and U-87MG cell lines. These synthesized materials hold immense BNCT promise, boasting minimal toxicity and striking anti-tumor efficacy that transcends established clinical counterparts, potentially revolutionizing tumor diagnosis and therapy.