CuO-CeO₂ nanocatalysts with varying CuO contents (1, 5, 9, 14 and 17 wt %) were prepared by one-step flame spray pyrolysis (FSP) and applied to CO oxidation. The influences of CuO content on the as-prepared catalysts were systematically characterized by X-ray diffraction (XRD), N₂ adsorption-desorption at −196 °C, field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and hydrogen-temperature programmed reduction (H₂-TPR). A superior CO oxidation activity was observed for the 14 wt % CuO-CeO₂ catalyst, with 90% CO conversion at 98 °C at space velocity (60,000 mL × g⁻¹ × h⁻¹), which was attributed to abundant surface defects (lattice distortion, Ce³⁺, and oxygen vacancies) and high reducibility supported by strong synergistic interaction. In addition, the catalyst also displayed excellent stability and resistance to water vapor. Significantly, in situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS) showed that in the CO catalytic oxidation process, the strong synergistic interaction led readily to dehydroxylation and CO adsorption on Cu⁺ at low temperature. Furthermore, in the feed of water vapor, although there was an adverse effect on the access of CO adsorption, there was also a positive effect on the formation of fewer carbon intermediates. All these results showed the potential of highly active and water vapor-resistive CuO-CeO₂ catalysts prepared by FSP.

Rational design LDHs (layered double hydroxides) with 3D hierarchical hollow structures have generated widespread interest for catalytic oxidation due to the high complexity in shell architecture and composition. Herein, we reported a handy two-step method to construct a 3D hierarchical NiCo₂O₄/NiO nanocage. This synthetic strategy contains a partial in situ transformation of ZIF-67 (zeolitic imidazolate framework-67) into Co-NiLDH yolk-shelled structures following ethanol etching, and a structure-preserved transformation from Co-NiLDH@ZIF-67 to a biphase nanocage following calcination. CoNi-yh-T (varied reaction time and calcination temperature) nanocages were investigated systematically by Brunauer–Emmett–Teller (BET), X-ray photoelectron spectroscopy (XPS), H₂- temperature-programmed reduction (TPR), NH₃-temperature-programmed desorption (TPD) and studied for toluene oxidation. The CoNi-6h-350 sample showed much higher activity with 90% toluene conversion (T₉₀) at 229 °C at a high space velocity (SV = 60,000 mL g⁻¹ h⁻¹) than other catalysts (T₉₀ >240 °C). Abundant surface high valence Co ions caused by the novel hierarchical nanostructures, together with adsorbed oxygen species and abundant medium-strength surface acid sites, played a key role for catalytic activities.