Designing sensing materials with novel morphologies and compositions is eminently challenging to achieve high-performance gas sensor devices. Herein, an in situ oxidative polymerization approach is developed to construct three-dimensional (3D) hollow quasi-graphite capsules/polyaniline (GCs/PANI) hierarchical hybrids by decorating protonated PANI on the surface of GCs; as a result, an immensely active and sensitive material was developed for sensing ammonia gas at room temperature. Moreover, the GCs possessed a capsule-like hollow/open structure with partially graphitized walls, and PANI nanospheres were uniformly decorated on the GC surfaces. Furthermore, the inflexible and rigid 3D ordered chemistry of these materials provides the resulting hybrids with a large interfacial surface area, which not only allows for rapid adsorption and charge transfer but also provides the necessary structural stability. The 3D hollow GCs/PANI hybrids exhibit excellent performance; the GCs/PANI-3 hybrid is highly sensitive (with a response value of 1.30) toward 10 ppm NH 3 gas and has short response and recovery times of 34 and 42 s, respectively. The GCs/PANI-3 hybrid also demonstrates a good selectivity, repeatability, and long-term stability, which are attributed to the substantial synergistic effect of the GCs and PANI. The design of such a unique 3D ordered framework provides a promising pathway to achieve room-temperature gas sensors for commercial applications.

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