Unique porous ZnO polygonal nanoflakes were synthesized by the microwave hydrothermal method. The structural properties of the products were investigated by using X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), and high-resolution TEM techniques. In situ diffuse reflectance infrared Fourier transform spectroscopy technique was employed to investigate the mechanism of NO2 sensing. Free nitrate ions, nitrate ions, and nitrite anions were the main adsorbed species. N2O was formed via NO– and N2O2 – that were stemmed from NO. Comparative tests for gas sensing between gas sensors based on the as-prepared porous ZnO nanoflakes and purchased ZnO nanoparticles clearly showed that the former exhibited more excellent NO2 sensing performances. Photoluminescence and X-ray photoelectron spectroscopy spectra further proved that the intensities of donors (oxygen vacancy (VO) and/or zinc interstitial (Zni)) and surface oxygen species (O2 – and O2), which were involved in the mechanism of gas sensing led to the different gas-sensing properties.

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