Developing a high performance sensing materials operating at room temperature (30 °C) is eminently a challenging task. The facile chemical oxidative polymerization route was employed for the synthesis of PAni‐CeO2 nanohybrids with CSA intercalation (10–50 wt %) on the chains of protonated PAni. The cubic crystal structure of PAni‐CeO2‐CSA nanohybrids were revealed by X‐ray diffractometry (XRD). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were employed for the structural and morphological investigations. X‐ray Photoelectron Spectroscopy (XPS) and Raman spectroscopy confirmed the formation of PAni‐CeO2‐CSA nanohybrid. The consequences of CSA intercalation on the gas sensing performance of PAni‐CeO2 nanohybrids are explored through custom designed sensing system. The gas sensing investigations revealed that PAni‐CeO2‐CSA (50 wt %) nanohybrid exhibited highest response (93 %) towards 100 ppm NH3 at 30 °C. Advantageously, CSA intercalated PAni‐CeO2 nanohybrid gas sensor delivered fast response and quick recovery (8 sec and 482 sec) with admirable stability (84.09 %) towards NH3 at 30 °C.
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