Titanium dioxide (TiO 2 ) nanorods in the brookite phase, with average dimensions of 3–4 nm × 20–50 nm, were synthesized by a wet-chemical aminolysis route and used as precursors for thin films that were deposited by the matrix-assisted pulsed laser evaporation (MAPLE) technique. A nanorod solution in toluene (0.016 wt% TiO 2 ) was frozen at the liquid-nitrogen temperature and irradiated with a KrF excimer laser at a fluence of 350 mJ/cm 2 and repetition rate of 10 Hz. Single-crystal Si wafers, silica slides, carbon-coated Cu grids and alumina interdigitated slabs were used as substrates to allow performing different characterizations. Films fabricated with 6000 laser pulses had an average thickness of ∼150 nm, and a complete coverage of the selected substrate as achieved. High-resolution scanning and transmission electron microscopy investigations evidenced the formation of quite rough films incorporating individually distinguishable TiO 2 nanorods and crystalline spherical nanoparticles with an average diameter of ∼13 nm. Spectrophotometric analysis showed high transparency through the UV-Vis spectral range. Promising resistive sensing responses to 1 ppm of NO 2 mixed in dry air were obtained.