Carbon disulfide (CS2), a highly toxic volatile sulfur-containing industrial gas, poses serious risks to industrial safety, occupational health, and the environment, creating an urgent demand for highly sensitive and reliable detection. In this work, hierarchical ZnO/Fe2O3 nanomaterials were synthesized via the pyrolysis of a nanosized ZIF-8 precursor for CS2 detection. The optimized nanoheterostructures exhibited superior CS2-sensing performance compared with their single-component counterparts, benefiting from efficient interfacial charge modulation within the n–n nanoheterojunctions and abundant active sites provided by the hierarchical nanoarchitecture. The optimized ZnO/Fe2O3 sensor enabled highly sensitive CS2 detection with a theoretical LOD of 0.66 ppm. To suppress humidity-induced signal fluctuations, a CSA-optimized CatBoost model was developed for humidity compensation and achieved the highest prediction accuracy among the multiple metaheuristic optimization strategies. This work provides an effective strategy for the rational design of hierarchical nanoheterostructures with enhanced gas-sensing performance and demonstrates an intelligent humidity compensation approach for reliable CS2 detection under practical operating conditions.
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