Abstract: | The two‐dimensional (2D) vanadium carbide (V2C) MXene has shown great potential as a photothermal agent (PTA) for photothermal therapy (PTT). However, the use of V2C in PTT is limited by the harsh synthesis condition and low photothermal conversion efficiency (PTCE). Herein, we report a completely different green delamination method using algae extraction to intercalate and delaminate V2AlC to produce mass V2C nanosheets (NSs) with a high yield (90 %). The resulting V2C NSs demonstrated good structural integrity and remarkably high absorption in near infrared (NIR) region with a PTCE as high as 48 %. Systemic in vitro and in vivo studies demonstrate that the V2C NSs can serve as efficient PTA for photoacoustic (PA) and magnetic resonance imaging (MRI)‐guided PTT of cancer. This work provides a cost‐effective, environment‐friendly, and high‐yielding disassembly approach of MAX, opening a new avenue to develop MXenes with desirable properties for a myriad of applications. |