The growing hydrogen industry is stimulating an ongoing search for new materials not only for hydrogen production or storage but also for hydrogen sensing. These materials have to be sensitive to hydrogen, but additionally, their synthesis should be compatible with the microcircuit industry to enable seamless integration into various devices. In addition, the interference of air humidity remains an issue for hydrogen sensing materials. We approach these challenges using conventional reactive sputter deposition. Using three consequential processes, we synthesized multilayer structures. A basic two-layer system composed of a base layer of cupric oxide (CuO) overlayered with a nanostructured copper tungstate (CuWO₄) exhibits higher sensitivity than individual materials. This is explained by the formation of microscopic heterojunctions. The addition of a third layer of palladium oxide (PdO) in forms of thin film and particles resulted in a reduction in humidity interference. As a result, a sensing three-layer system working at 150 °C with an equalized response in dry/humid air was developed.

By tuning the deposition parameters of reactive high-power impulse magnetron sputtering, specifically the pulse length, we were able to prepare WO_3−x films with various stoichiometry and structure. Subsequently, the films were annealed in air at moderate temperature (350 °C). We demonstrate that the stoichiometry of the as-deposited films influences considerably the type of crystalline phase formed in the annealed films. The appropriate sub-stoichiometry of the films (approx. WO_2.76) enabled crystallization of the monoclinic phase during the annealing. This phase is favorable for hydrogen sensing applications. To characterize the sensory behavior of the films, the tungsten oxide films were decorated by Pd nanoparticles before annealing and were assembled as a conductometric gas sensor. The sensory response of the films that crystallized in the monoclinic structure was proven to be superior to that of the films containing other phases.