| Summary: | The major drawback of oxide-based sensors is the lack of selectivity. In this context, Sn<sub>x</sub>Ti<sub>1−x</sub>O<sub>2</sub>/graphene oxide (GO)-based materials were synthesized via a simple hydrothermal route, varying the titanium content in the tin dioxide matrix. Then, toluene and acetone gas sensing performances of the as-prepared sensors were systematically investigated. Specifically, by using 32:1 SnO<sub>2</sub>/GO and 32:1 TiO<sub>2</sub>/GO, a greater selectivity towards acetone analyte, also at room temperature, was obtained even at ppb level. However, solid solutions possessing a higher content of tin relative to titanium (as 32:1 Sn<sub>0.55</sub>Ti<sub>0.45</sub>O<sub>2</sub>/GO) exhibited higher selectivity towards bigger and non-polar molecules (such as toluene) at 350 °C, rather than acetone. A deep experimental investigation of structural (XRPD and Raman), morphological (SEM, TEM, BET surface area and pores volume) and surface (XPS analyses) properties allowed us to give a feasible explanation of the different selectivity. Moreover, by exploiting the UV light, the lowest operating temperature to obtain a significant and reliable signal was 250 °C, keeping the greater selectivity to the toluene analyte. Hence, the feasibility of tuning the chemical selectivity by engineering the relative amount of SnO<sub>2</sub> and TiO<sub>2</sub> is a promising feature that may guide the future development of miniaturized chemoresistors.
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