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.

The influence of high indoor humidity on building and equipment safety and human health has led to an urgent demand for the development of high‐performance dehumidification technologies. To simultaneously satisfy the requirements of easy shaping, nontoxicity, and low energy consumption for indoor dehumidification, an effective strategy involving the combination of non‐toxic microporous materials with a shaping matrix equipped with switching functionalities via a synergetic porous interface can be used. This study proposes an in situ interface‐controlled growth method to produce a novel hierarchically porous hydrogel adsorbent for indoor dehumidification by combining metal–organic frameworks (MOFs) with a poly(N‐isopropylacrylamide) (PNIPAM) thermoresponsive hydrogel matrix. The obtained composite hydrogel monolith, ThermoGel‐23, exhibits a moisture uptake capacity of 1.64 g·g ⁻¹ , high adsorption rate, and desorption activation energy as low as 31.0 kJ·mol ⁻¹ , meeting the requirements of indoor adsorption dehumidification. Combining experiments and simulations, we elucidated the transport pathways of water clusters within the hierarchical pores and highlighted the essential role of porous structure and thermal response in enhancing both adsorption and desorption. This work demonstrates the potential of MOF–polymer composites as efficient, scalable desiccants, paving the way for sustainable and energy‐saving humidity control materials.