Highly Responsive Pd-Decorated MoO₃ Nanowall H₂ Gas Sensors Obtained from In-Situ-Controlled Thermal Oxidation of Sputtered MoS₂ Films

Among transition metal oxides, MoO₃ is a promising material due to its layered structure and different oxidation states, making it suitable for different device applications. One of the methods used to grow MoO₃ is radio frequency magnetron sputtering (RFMS), which is the most compatible method in industry. However, obtaining nanostructures by RFMS for metal oxides is challenging because of compact morphology film formation. In this study, α-MoO₃ with vertical nanowalls is obtained by a two-step process; deposition of magnetron-sputtered MoS₂ vertical nanowalls and postoxidation of these structures without changing the morphology. In situ transmittance and electrical measurements are performed to control the oxidation process, which shed light on understanding the oxidation of MoS₂ nanowalls. The transition from MoS₂ to α-MoO₃ is investigated with partially oxidized MoS₂/MoO₃ samples with different thicknesses. It is also concluded that oxidation starts from nanowalls perpendicular to the substrate and lasts with oxidation of basal planes. Four different thicknesses of α-MoO₃ nanowall samples are fabricated for H₂ gas sensors. Also, the effect of Pd deposition on the H₂-sensing properties of sensors is deeply investigated. An outstanding response of 3.3 × 10⁵ as well as the response and recovery times of 379 and 304 s, respectively, are achieved from the thinnest Pd-loaded sample. Also, the gas-sensing mechanism is explored by gasochromic measurements to investigate the sensor behaviors under the conditions of dry air and N₂ gas as the carrier gas.