Here, we report a novel metal-organic framework ZIF-8based nanocomposite with encapsulated molybdenum disulfide(MoS₂)nanosheets and doxorubicin(DOX)for pH- and NIR-triggered synergistic chemo/photothermal treatment of cancer cells. First, MoS₂ nanosheets, which have uniform size of ~100 nm and topological height of 0.3~1.4 nm, are synthesized by hydrothermal reaction and ultrasonic treatment. Subsequently,an aciddegradable metalorganic framework ZIF-8 is employed to synchronously encapsulate MoS₂ nanosheets and anticancer drug DOX to obtain DOX loaded ZIF-8 coated MoS₂ (DOX/MoS₂@ZIF-8)nanocomposites by onestep method. The nanocomposites are used for chemo/photothermal synergistic treatment of cancer cells: under acid conditions (e.g. pH 5.0 in a lysosome)and NIR laser irradiation (780 nm, 2.1 W/cm²), the ZIF-8 of the DOX/MoS₂@ZIF-8 nanocomposites can be degraded, resulting in the release of encapsulated DOX, the cytosolic DOX can enter the nucleus to induce apoptosis. Meanwhile, the MoS₂ nanosheets can effectively convert NIR laser light energy into heat energy, the photoinduced hyperthermia can also induce apoptosis. Thus, chemo/photothermal synergistic cancer therapy is realized. Cell viability assays show that this DOX/MoS₂@ZIF-8 nanocomposites have an excellent chemo/photothermal synergistic treatment effect on SMMC7721 cells, which can kill the tumor cells efficiently.