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One-step single-spinneret electrospinning synthesis of 1D fibrous hierarchical structure can not only prevent the agglomeration or restacking of fibers or particles and enlarge surface active area but also promote the directional migration of electrons in materials and achieve effective regulation of resistances. Herein, tunable SnO 2 and SnO 2 /ZnO fibrous hierarchical structures with in situ growth of monodisperse spherical-like particles on surface provide a new sight for adjusting component distribution, surface absorption and chemical reaction, electronic transmission path, and electron transfer efficiency. Compared with SnO 2 porous fibers and SnO 2 hierarchical structures, the optimal SnO 2 /ZnO sensors exhibit superior gas-sensing response value of 366-100 ppm ethanol at 260 °C as well as excellent gas selectivity and long-term stability, in which the enhanced gas-sensing mechanism is primarily derived from multilevel effective heterojunctions with unique interface electronic effects. Especially, these SnO 2 -based sensors can achieve favorable linear relationship of the response and gas concentration for sensitive trace detection in cosmetics for the first time, providing a new strategy to design composite materials for quantitative analysis of volatiles in the cosmetics evaluation process.

Morphology-tunable C-N/SnO 2 -based hierarchical microspheres with good gas sensitivity for triethylamine (TEA) have been fabricated via facile electrospinning and a subsequent calcination process. The reaction temperature and modifying calcining technology played a dominant role for the morphological evolution from precursor fibers to microspherical shapes and the formation of C-N-decorated SnO 2 phase composition. C-N/SnO 2 /ZnO composites with tunable crystallinity, microstructure, and gas-sensing performance were strictly dependent on the added amount of Zn element. Fascinatingly, the constructed C-N/SnO 2 /ZnO/Au composites can not only precisely regulate the crystal size, dispersion status, loading position, and content of Au nanoparticles but also display excellent gas-sensing properties with ultrasensitivity and high selectivity under various temperature detections. The response of C-N/SnO 2 /ZnO/Au composites can reach up to approximately 1970, calculated to be 121.6 and 23.6 times for 50 ppm TEA molecules at optimal conditions compared with C-N/SnO 2 and C-N/SnO 2 /ZnO microspheres, respectively, actually representing the highest response value at high temperatures reported to date. The superior long-aging stability of sensing behaviors and phase structures can be also observed after 1 month. More importantly, novel C-N/SnO 2 /ZnO/Au sensors were employed for availably detecting low-concentration volatiles released from the storage procedure of fishes at 80 °C, indicating the practical application in chemical detectors and biosensors at low temperature. The novel gas-sensing mechanisms derived primarily from the combination of phase compositions, morphologies, and unique surface/interface transfer processes of C-N/SnO 2 /ZnO/Au composites are presented and investigated in detail, which will contribute to the design and development of other semiconductor-based composite sensors.