This study investigates the impact of two distinct methodologies on the structural, morphological, and gas sensing properties of TiO2/SiC/CoFe2O4 (TSC) nanocomposites determined using x-ray diffraction (XRD), scanning electron microscopy (SEM), LCR meter, and gas sensing unit respectively. The TiO2/SiC/CoFe2O4 nanocomposites were synthesized using chemical co-precipitation method (C-TSC) and the solid state method (G-TSC). The Scherrer formula was used to calculate the average grain size of C-TSC and G-TSC, which was estimated to be 8 ± 2 nm and 10 ± 2 nm, respectively. The formation of TSC nanocomposites was confirmed by XRD, SEM, and EDX analysis. The response (%) toward ethanol and NH3 gas was tested as a function of flow rate (ppm) and temperature from room temperature (28 °C) to 300 °C. The response (%) was observed to be increasing with increasing temperature and three intermediate temperatures were found. The response and recovery time were also measured with varying gas concentrations. The long-term stability of devices was tested up to 30 days and less variation in result was found, which confirms stability of sensor. The material synthesized using chemical co-precipitation method (C-TSC) shows better properties than G-TSC.