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Polypyrrole (PPy) nanorods (NRs) and nanoparticles (NPs) are synthesized via electrochemical and chemical methods, respectively, and tested upon ammonia exposure using Raman and X-ray photoelectron spectroscopy (XPS). Characterization of both nanomaterials via Raman spectroscopy demonstrates the formation of PPy, displaying vibration bands consistent with the literature. Additionally, XPS reveals the presence of neutral PPy species as major components in PPy NRs and PPy NPs, and other species including polarons and bipolarons. Raman and XPS analysis after ammonia exposure show changes in the physical/chemical properties of PPy, confirming the potential of both samples for ammonia sensing. Results demonstrate that the electrochemically synthesized NRs involve both proton and electron transfer mechanisms during ammonia exposure, as opposed to the chemically synthesized NPs, which show a mechanism dominated by electron transfer. Thus, the different detection mechanisms in PPy NRs and PPy NPs appear to be connected to the particular morphological and chemical composition of each film. These results contribute to elucidate the mechanisms involved in ammonia detection and the influence of the synthesis routes and the physical/chemical characteristics of PPy.

This review summarizes the recent research efforts and developments in nanomaterials for sensing volatile organic compounds (VOCs). The discussion focuses on key materials such as metal oxides (e.g., ZnO, SnO2, TiO2 WO3), conductive polymers (e.g., polypyrrole, polythiophene, poly(3,4-ethylenedioxythiophene)), and carbon-based materials (e.g., graphene, graphene oxide, carbon nanotubes), and their mutual combination due to their representativeness in VOCs sensing. Moreover, it delves into the main characteristics and tuning of these materials to achieve enhanced functionality (sensitivity, selectivity, speed of response, and stability). The usual synthesis methods and their advantages towards their integration with microsystems for practical applications are also remarked on. The literature survey shows the most successful systems include structured morphologies, particularly hierarchical structures at the nanometric scale, with intentionally introduced tunable “decorative impurities” or well-defined interfaces forming bilayer structures. These groups of modified or functionalized structures, in which metal oxides are still the main protagonists either as host or guest elements, have proved improvements in VOCs sensing. The work also identifies the need to explore new hybrid material combinations, as well as the convenience of incorporating other transducing principles further than resistive that allow the exploitation of mixed output concepts (e.g., electric, optic, mechanic).