In-situ monitoring of tungsten oxides reduction during deuterium plasma exposure by spectroscopic ellipsometry

In this work, we investigate the optical properties variation of thermally grown W oxides during the exposure to low energy deuterium (D) plasma. In-situ ellipsometry in the 400–1000 nm range was coupled to ex-situ diagnostics, such as X-ray photoelectron spectroscopy (XPS) and focused ion beam coupled to scanning electron microscopy (FIB-SEM), to probe the evolution of chemical and morphological properties of the W oxides. First, a 70 nm thick $W{O}_3$ layer was exposed to D plasma at a surface temperature of 650 K. An important reduction of the oxide layer was observed by FIB-SEM, and in-situ ellipsometry showed the evolution of the optical constants n and k of the oxide towards the ones of pure W metal. Secondly, a 300 nm thick $W{O}_3$ layer was exposed to D plasma at a surface temperature below 373 K. In order to follow the oxide evolution step by step, we alternated in-situ ellipsometry and XPS surface characterization. A quite similar evolution of the optical constants was observed, in particular an increase of the extinction coefficient k in the near infrared, which was linked to a progressive reduction of the oxidation level at the surface, as seen by XPS. Interestingly, the reduction of the oxide at 373 K was below the resolution of the FIB-SEM. This observation indicates that ellipsometry in the 400–1000 nm range is able to follow in-situ the reduction of $W{O}_3$ oxides by D plasma with high surface sensitivity.