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Facile preparation of multifunctional theranostic nanoplatforms with well-controlled morphology and sizes remains an attractive in the area of nanomedicine. Here, a new kind of 2D transition metal dichalcogenide, rhenium disulfide (ReS2) nanosheets, with uniform sizes, strong near-infrared (NIR) light, and strong X-ray attenuation, is successfully synthesized. After surface modification with poly(ethylene glycol) (PEG), the synthesized ReS2-PEG nanosheets are stable in various physiological solutions. In addition to their contrasts in photoacoustic imaging and X-ray computed tomography imaging because of their strong NIR light and X-ray absorptions, respectively, such ReS2-PEG nanosheets can also be tracked under nuclear imaging after chelator-free labeling with radioisotope ions, 99mTc4+. Efficient tumor accumulation of ReS2-PEG nanosheets is then observed after intravenous injection into tumor-bearing mice under triple-modal imaging. The combined in vivo photothermal radiotherapy is further conducted, achieving a remarkable synergistic tumor destruction effect. Finally, no obvious toxicity of ReS2-PEG nanosheets is observed from the treated mice within 30 d. This work suggests that such ultrathin ReS2 nanosheets with well-controlled morphology and uniform sizes may be a promising type of multifunctional theranostic agent for remotely triggered cancer combination therapy. [ABSTRACT FROM AUTHOR]