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Ti₃C₂ MXene is a new two-dimensional material exhibiting a variety of novel properties including good photothermal effect, and the capability of Ti₃C₂ for multimodal tumor therapy is in urgent need of development. Herein, ultrathin Ti₃C₂ MXene nanosheets (∼100 nm) have been synthesized by supplying additive Al³⁺ to avoid Al loss and employed as a photothermal/photodynamic agent for cancer therapy. The as-obtained nanosheets exhibit outstanding mass extinction coefficient (28.6 Lg^–1 cm^–1 at 808 nm), superior photothermal conversion efficiency (∼58.3%), and effective singlet oxygen generation (¹O₂) upon 808 nm laser irradiation. Based on these Ti₃C₂ nanosheets, a multifunctional nanoplatform (Ti₃C₂-DOX) is established via layer-by-layer surface modification with doxorubicin (DOX) and hyaluronic acid (HA). In vitro and in vivo experiments disclose that Ti₃C₂-DOX shows enhanced biocompatibility …