Multicomponent spinel ferrites are essential to be used in high-performance gas-sensing materials. Herein, multinary (Cu,Zn)Fe2O4 spinel nano-microspheres with tunable internal structures, including solid, core-shell, and yolk-shell, were successfully synthesized by a simple self-templated solvothermal method combined with a subsequent annealing strategy. The internal structures of the (Cu,Zn)Fe2O4 nano-microspheres significantly rely on the heating rates of the precursors, which show promising selective response towards trimethylamine gas. Among them, the as-formed yolk-shell (Cu,Zn)Fe2O4 nano-microspheres exhibited high response to triethylamine with excellent selectivity of STEA/SX = 1.86 at 160 °C, fast response-recovery rate (58 s/136 s), and long-term repeatability and stability of more than one month. The corresponding triethylamine gas-sensing mechanism with the special microstructures is discussed. This work provides new insights into the rational design of interior structure and the modulation of high gas response and selectivity of multinary spinel ferrites in gas-sensing applications.
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