A new active layer for CO 2 sensing based on semiconducting CuO–Cu x Fe 3− x O 4 (with 0 ≤ x ≤ 1) nanocomposite was prepared by radiofrequency sputtering from a delafossite CuFeO 2 target using a specific in situ reduction method followed by post annealing treatment in air. The tenorite–spinel ferrite nanocomposite layer was deposited on a simplified test device and the response in a carbon dioxide atmosphere was measured by varying the concentration up to 5000 ppm, at different working temperatures (130–475 °C) and frequencies (0.5–250 kHz). The results showed a high response of 50% ( R air / R C O 2 = 1.9 ) at 250 °C and 700 Hz for a CO 2 concentration of 5000 ppm.