This paper reports on the in situ analysis of nickel silicide (NiSi) thin films formed by thermal processing of nickel thin films deposited on silicon substrates. The in situ techniques employed for this study include micro-Raman spectroscopy (μRS) and X-ray diffraction (XRD); in both cases the variations for temperatures up to 350 ºC has been studied.

Nickel silicide thin films formed by vacuum annealing of nickel on silicon (at 350 ºC for 30 minutes) were used as a reference for measurements. These silicide thin films have been studied using Auger electron spectroscopy depth profiles to verify the 1:1 nickel to silicon stoichiometry and glancing angle X-ray diffraction to determine the crystal orientation. Micro-Raman analysis results for these films are reported, indicating very low stress in the films, evident from a null shift of the major 214 cm^-1 peak (compared to the spectra for NiSi powder).

In situ analysis was carried out on nickel thin films on silicon, while the samples are heated from room temperature to 350 ºC. Data was gathered at regular temperature intervals (in steps of 25-50 ºC) and other specific points of interest (such as 250 ºC, where the reaction between nickel and silicon to form Ni₂Si is expected). The transformations from the metallic state, through the intermediate reaction states, until the desired metal-silicon reaction product is attained are discussed. The evolution of nickel silicide from the nickel film can be observed from both the μRS and XRD in situ studies. Variations in the evolution of silicide from metal for different silicon substrates are discussed, and these include (100) n-type, (100) p-type, and (110) p-type silicon substrates.

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