Conventional cancer therapies such as radiation, surgery, and chemotherapy have demonstrated effectiveness in eradicating tumor tissues. However, it is accompanied with adverse side effects and risk of tumor recurrence in patients. Near infrared (NIR)-based phototherapies such as Photothermal (PTT) and photodynamic (PDT) therapy for cancer have an incomparable advantage over the conventional treatments in precisely eradicating unresectable tumors without affecting healthy tissues. Furthermore, the approach is minimally invasive and maximal tumor eradication can be achieved by locally irradiating the tumor using NIR laser. The generation of heat or reactive oxygen species to kill the cancer cells are dictated by the concentration of photosensitizer accumulated in the tumor. Nanomaterial-based photosensitizers offers a possible to enhance the phototherapy by specifically targeting and accumulating in the tumor region. The objective of this Methods Collection is to share optimized protocols for synthesis, characterization, and explore the application of nanomaterial-based photosensitizers for cancer phototherapy.