Multi-technique Approach for the Evaluation of the Crystalline Phase of Ultrathin High-k Gate Oxide Films

In order to continue scaling metal oxide semiconductor field effect transistors (MOSFETs) with HfO2 gate oxides, efforts are being made to further improve the deposited high-k film properties. Recently, a process whereby an HfO2 film is deposited through a series of depositions and anneals (so-called DADA process) has been shown to result in films that give rise to MOS capacitors (MOSCAPs) which are electrically scaled compared to MOSCAPs with HfO2 films that only received post deposition anneals (PDA) or no anneals. We have measured as-deposited, DADA and PDA HfO2 films using four measurement techniques, all of which are non-destructive and capable of being used for in-line processing, to evaluate their crystallinity and crystalline phases. Grazing incidence in-plane X-ray diffraction was used to determine the crystalline phases of the HfO2 films. We observed the crystalline phases of these films to be process dependent. Additionally, X-ray and UV photoelectron spectroscopy were used to show the presence of crystallinity in the films. As a fourth technique, spectroscopic ellipsometry was used to determine if the crystalline phases were monoclinic. The combination of techniques was useful in that XPS and UPS were able to confirm the amorphous nature of a 30 cycle DADA film, as measured by GIIXRD, and GIIXRD was able to help us interpret the SE data as being an indication of the monoclinic phase of HfO2.