Abstract: | In the present paper, suitable TiO2 nanoparticles are successfully synthesized by sol‐gel method, in order to utilize the freshly prepared TiO2 nanoparticles for proton exchange membrane (PEM) preparation. Titanium tetrachloride (TiCl4) is used as precursor and ethanol as a solvent. The optimum and suitable TiO2 nanoparticles were obtained by varying gelatinisation time (4–120 h), concentration of precursor (TiCl4) in ethanol (2–15 vol%), and reaction temperature (15–35 °C). The morphology, size and purity of the nanoparticles are investigated by transmission electron microscope (TEM), dynamic light scattering (DLS) and X‐ray diffraction (XRD). Optimum results were found at 4 h of gelatinisation time, 10% precursor concentration and 25 °C temperature for preparation of TiO2 nanoparticles. Thus prepared nanoparticles are found to be suitable for preparation of nanocomposite PEM, and consequently the prepared PEM indicates enhanced properties, such as, higher thermal stability (high glass transition temperature of 184.1 °C), excellent proton conductivity (0.0822 S cm−1 at room temperature) and low methanol permeability (1.11 × 10−9 cm2 s−1). |