〔Abstract〕 Objective To explore the application of ZnxNi1-xS@DOX nanostructures in combined photothermal-chemotherapy treatment of tumors, and to provide new ideas for the study of tumor treatment methods. Methods The morphology and elementary composition of ZnxNi1-xS nanostructures were characterized by scanning emission electron microscopy and other methods. The photothermal properties of ZnxNi1-xS nanostructures were explored by infrared thermal camera. The release of DOX under different temperature and pH was investigated by fluorescence spectrophotometer. The biosafety of ZnxNi1-xS nanostructures and thein vitroantitumor properties of ZnxNi1-xS@DOX nanostructures were investigated by MTT assay. Results The as-prepared ZnxNi1-xS nanostructure had good dispersion and uniform size. The ZnxNi1-xS nanostructures had good photothermal effect. The drug release behavior showed temperature and pH responsiveness. The MTT assay showed that ZnxNi1-xS nanostructures were nontoxic to normal cells. ZnxNi1-xS@DOX nanostructures could significantly inhibit the growth of tumor cells under near-infrared illumination. Conclusion The as-prepared ZnxNi1-xS nanostructure has good biocompatibility, on the basis of which the ZnxNi1-xS@DOX nanostructures achieve good antitumor performance, which can be used for combined photothermal-chemotherapy treatment of tumors.