Depth-Profiling XPS Study of Oxygen Diffusion and Reduction During Low-Temperature Activation of Ti-Co-Ce Getter Films

In this study, Ti-Co-Ce getter films were deposited via magnetron sputtering to investigate their activation mechanism—the thermal removal of surface passivation layers to restore gas sorption capability. The morphology before and after film activation was characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM). The oxygen content on the film surface before and after activation was measured using an energy-dispersive X-ray spectrometer (EDS), and gas desorption during activation was monitored with a quadrupole mass spectrometer (QMS). The combined results confirmed the absence of O2 desorption during activation, suggesting oxygen migration into the film bulk. Crucially, in situ X-ray photoelectron spectroscopy (XPS) combined with controlled Ar+ ion sputtering depth profiling (0–30 nm) was employed to directly probe the chemical-state evolution within the thin film before and after thermal activation at 400 °C, thereby providing direct evidence of the activation dynamics. The data reveal that within the 0–10 nm near-surface region, a strong oxygen chemical potential gradient drives rapid oxide reduction and inward migration of lattice oxygen. At depths of 20–30 nm, moderate reduction coupled with oxygen enrichment induces phase separation, while around 30 nm, a dynamic equilibrium between oxygen inflow and outflow is established. These findings provide a theoretical basis for optimizing activation processes and guiding the development of low-temperature getter materials. This work is particularly relevant for MEMS, vacuum electronics, and other applications with stringent thermal budgets, expanding the design possibilities for heat-sensitive device integration.