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The Xikuangshan antimony (Sb) deposit is the world’s largest known Sb deposit. Due to the lack of suitable minerals for reliable high-precision radiometric dating, it remains difficult to determine the exact age of Sb mineralization in this deposit. Here, we report the first LA-MC-ICP-MS U-Pb ages of syn-stibnite calcite from this deposit. The dating results indicate the presence of at least two stages of Sb mineralization in the Xikuangshan ore district. The calcite-stibnite veins in the Daocaowan ore block probably formed during the Paleocene (58.1 ± 0.9 Ma), representing an early stage of Sb mineralization, while the quartz-stibnite vein in the Feishuiyan ore block probably formed during the Eocene (50.4 ± 4.4 Ma, 50.4 ± 5.0 Ma, and 51.9 ± 1.6 Ma), representing a late stage of Sb mineralization. The new calcite U-Pb ages are significantly younger than the calcite Sm-Nd ages (124.1 ± 3.7 Ma, 155.5 ± 1.1 Ma) reported by previous researchers. We suggest that Sb mineralization of the South China antimony metallogenic belt may be related to tectono-thermal events during Paleogene, possibly linked to high heat flow during the subduction (ca. 60–40 Ma) of the Pacific Plate beneath the Eurasian Plate and/or the Indo–Asian Collision (began at ca. 61 Ma). The young in situ U-Pb ages of calcite challenge the idea of late Mesozoic Sb mineralization in the South China antimony metallogenic belt, suggesting the requirement for more high-precision dating studies.

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The Daocaowan antimony (Sb) deposit is a newly discovered Sb deposit located outside the northeast Xikuangshan ore field. In the absence of geochemical data, the metallogenic mechanism of the Daocaowan Sb deposit and its relationship with the Xikuangshan ore field remains unclear. Using high-resolution LA-ICP-MS technique, this study quantitatively determined the in-situ S isotope values and trace element composition of stibnite from the Daocaowan Sb deposit in South China to investigate the source of ore-forming materials and genesis of this deposit. The trace element compositions of stibnite from the Daocaowan Sb deposit revealed the form of occurrence and substitution mechanism of trace elements in stibnite, providing new constraints for explaining the genesis of Sb deposits. The relatively smooth LA-ICP-MS profiles indicate that As, Cu, Hg, and Pb primarily occur as solid solutions in stibnite. Therefore, we speculate that the substitution 3Sb3+↔As3+ + 2Cu+ + Hg2+ + Pb2+ may be the reason for the enrichment of As, Cu, Hg, and Pb in stibnite. A comparison with the Xikuangshan Sb deposit reveals the metallogenic mechanism of the Daocaowan Sb deposit, and the relationship between the two. With the exception of higher content of Fe in Stibnite from the Daocaowan deposit as compared to the Xikuangshan deposit, other trace elements are similar between the two deposits. The results show that the Daocaowan and Xikuangshan Sb deposits may have the same source of ore-forming fluids. We propose that the ore-forming fluid flowed through the Xikuangshan Sb deposit along the F75 fault and dissolved pyrite in the wall rock. Subsequently this fluid containing a high concentration of Fe precipitated and mineralized at Daocaowan. Meanwhile, the S isotope value of the Daocaowan Sb deposit (+6.65 to +9.29‰) is consistent with that of the Xikuangshan, proving that the ore-forming materials of the two deposits are from the same source, probably the basement strata. We propose that the Daocaowan Sb deposit is part of the Xikuangshan ore field, indicating a great prospecting potential in the northeast of the Xikuangshan ore field.