High specific surface area (SSA) nanocrystalline powders and dip-coated TiO 2 thin films have been prepared by a particulate sol–gel route with added polymeric fugitive agents (PFAs), namely trehalose dihydrate (THD), polyethylene glycol (PEG6000) and hydroxypropyl cellulose (HPC). One of the highest SSA reported in the literature, obtained without PFA, was achieved (i.e., 181m 2 /g), a value that could be increased up to 304m 2 /g, 274m 2 /g and 200m 2 /g for PEG/TiO 2 , HPC/TiO 2 and THD/TiO 2 powders, respectively. Furthermore, the crystallite size varied from 1nm for as-produced powders up to 4nm for powders heat-treated at 600°C. Thin films produced under optimised conditions showed excellent microstructural properties for gas sensing applications. They exhibited a stable and reproducible response towards CO and NO 2 at a low operating temperature of 200°C. Calibration curves revealed that all sensors followed the power law (S=A[gas] B ) (where S is sensor response, and coefficients A and B are constants) for the two kinds of gases and they have good capability for the detection of low gas concentrations (25ppm CO and 0.5ppm NO 2 ). Amongst all sensors, HPC/TiO 2 sensor showed the highest response towards CO≤100ppm and NO 2 ≤2ppm, whereas PEG/TiO 2 sensor had the highest response towards CO>100ppm and NO 2 >2ppm operated at 200°C. The response of the sensors to both CO and NO 2 changed with operating temperature reaching a maximum at a specific temperature. Moreover, the sensor response decreased by increasing the film annealing temperature. The response magnitude and response time of the sensors obtained in this work are superior to those reported in previous studies. Furthermore, their low power consumption as a result of their low operating temperature manifests their good potential for industrial application.