Breast cancer, particularly triple-negative breast cancer (TNBC), is the most impactful cancer affecting women, necessitating continuous evaluation of enhanced treatment methods. In this study, we synthesized a folic acid-modified gold nanoparticle-MoSe2 composite (FAM) by liquid exfoliation using glycyrrhizic acid (GA), spontaneous reduction of AuNP, and linkage between folic acid and AuNP using EDC/NHS coupling. With the assistance of GA, MoSe2 nanosheets can be easily exfoliated in aqueous solutions and exhibit biocompatibility. In addition, the gold nanoparticle deposition on the nanosheet was spontaneously induced due to the electron transfer property of MoSe2. Folic acid was used as a targeting molecule because triple-negative breast cancer (TNBC) lacks the common breast cancer markers. We investigated the effectiveness of photothermal therapy using FAM, which enhances light-heat transfer through the synergistic effect of gold and GA-exfoliated MoSe2 (GM). The nanomaterials exhibited improved photothermal conversion efficiency of 62.2 %, high thermal stability, and increased cellular uptake ratio. Subsequently, when the FAM reached the tumor microenvironment, the materials successfully entered the cells through folate receptor-mediated endocytosis and generated heat to kill cells under an 808 nm laser (0.8 W cm−2) by apoptosis. The biocompatibility and photothermic activity of FAM were determined in vitro by a tetrazolium salt assay, live/dead cell staining, cellular uptake ratio, and flow cytometry with human TNBC cells (MDA-MB-231). In summary, the FAM showed a more advanced therapeutic effect than GM in all outcomes. Our findings indicate that FAM has the potential to be used as a biomaterial for anticancer therapy.