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Single wavelength (670 nm laser diode) optical monitoring of reflectance at 1 second intervals was used to observe the
surface oxidation of Ni and Hafnium metal films in-situ in a low pressure oxygen atmosphere and also in a microwave
plasma oxygen environment.
After depositing thin metal films by sputtering in an oxygen-free environment, the observed reflectance quickly
decreased when low pressure oxygen gas was introduced into the vacuum chamber and reached a stable value within a
few seconds, after formation of a thin oxide layer. An additional rapid fall in reflectance and increase in oxide thickness
was observed when a microwave plasma generator was used to produce an oxygen plasma containing atomic oxygen.
Based on pre-determined optical properties of the metal and metal oxide films, the optical monitoring data was fitted to
obtain the thickness of the metal oxide as a function of time. The fitting results showed that the exposure to low pressure
oxygen forms an equilibrium thickness of less than 0.5 nm of NiOx and 0.78 nm of HfOx, while the oxygen microwave
plasma treatment produces an equilibrium thickness of 1.5 nm for both NiOx and HfOx.
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Shigeng Song, Frank Placido, "An in-situ investigation of the surface oxidation of ultra-thin films of Ni and Hf," Proc. SPIE 7101, Advances in Optical Thin Films III, 710120 (25 September 2008); https://doi.org/10.1117/12.803870