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Engineering of highly performing nanomaterials, capable of rapid detection of trace concentrations of gas molecules at room temperature, is key to the development of the next generation of miniaturized chemical sensors. Here, a highly performing nanoheterojunctions layout is presented for the rapid room‐temperature chemical sensing of volatile organic compounds down to ten particles per billion concentrations. The layout consists of a 3D network of nickel oxide–zinc oxide (NiO–ZnO) p–n semiconductors with grain size of ≈20 nm nanometers and a porosity of ≈98%. Notably, it is observed that the formation of the p–n heterojunctions by decoration of a ZnO nanoparticle networks with NiO increases the sensor response by more than four times while improving the lower limit of detection. Under solar light irradiation, the optimal NiO–ZnO nanoheterojunction networks demonstrate a strong and selective room‐temperature response to two important volatile organic compounds utilized for breath analysis, namely acetone and ethanol. Furthermore, these NiO–ZnO nanoheterojunctions show an inverse response to acetone from that observed for all others reducing gas molecules (i.e., ethanol, propane, and ethylbenzene). It is believed that these novel insights of the optoelectrochemical properties of ultraporous nanoheterojunction networks provide guidelines for the future design of low‐power solid‐state chemical sensors.

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Mechanochemical processing of anhydrous chloride precursors with Na2CO3 has been investigated as a means of manufacturing nanocrystalline SnO2 doped ZnO photocatalysts. High-energy milling and heat-treatment of a 0.1SnCl2+0.9ZnCl2+Na2CO3+4NaCl reactant mixture was found to result in the formation of a composite powder consisting of oxide grains embedded within a matrix of NaCl. Subsequent washing with deionized water resulted in removal of the NaCl matrix phase and partial hydration of the oxide reaction product with the consequent formation of ZnSn(OH)6. The extent of this hydration reaction was found to decrease in a linear fashion with the temperature of the post-milling heat-treatment over the range of 400–700 °C. For a heat-treatment temperature of 700 °C, the SnO2 doped ZnO powder was found to exhibit significantly higher photocatalytic activity than either single-phase SnO2 or ZnO powders that were synthesized using similar processing conditions. The heightened photocatalytic activity of the SnO2 doped ZnO was attributed to its higher specific surface area and the enhanced charge separation arising from the coupling of ZnO with SnO2.

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