A simple hydrothermal route to the synthesis of Sn-doped NiO hierarchical nanostructure is described in this paper. Gas sensors were fabricated from the as-prepared NiO nanostructures, and their gas sensing properties were investigated for response to various target gases. The results indicated that the sensor based on 3.0 at.% Sn-doped NiO nanospheres showed superior selectivity toward xylene, giving a response of 20.2–100 ppm, which was 12 times higher than that of the undoped NiO nanospheres. Moreover, this sensor based on the 3.0 at.% Sn-doped NiO hierarchical nanostructure had ppb-level detection limit that the response to 0.3 ppm xylene was 1.2. The likely reason for the improved sensing properties is the change of carrier concentration and chemisorbed oxygen amount caused by the implantation of Sn ions in NiO nanostructures.
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