The performance at room temperature of nanostructured polyaniline (PANi)–titanium dioxide (TiO₂) ammonia gas sensors was investigated. The PANi– TiO₂ thin-film sensors were fabricated with a spin-coating method on glass substrates. PANi–TiO₂ (0–50%) sensor films were characterized for their structural, morphological, optical, and various gas-sensing properties. The structural analysis showed the formation of nanocrystalline TiO₂, whereas PANi exhibited an amorphous nature. Morphological analysis of the PANi–TiO₂ nanocomposites film revealed a uniform distribution of TiO₂ nanoparticles in the PANi matrix. The absorption peaks in the Fourier transform infrared spectra and ultraviolet–visible spectra of the PANi–TiO₂ composite film were found to shift to higher wave numbers compared to those observed in pure PANi. The observed shifts were attributed to the interaction between the TiO₂ particles and the PANi molecular chains. The gas-sensing properties showed that the sensors exhibited selectivity to ammonia (NH₃) at room temperature.