The crystallization of ultrathin hafnium silicon oxynitride (HfSiON) gate dielectric is studied as a function of physical thickness. Grazing incidence x-ray diffraction (GI-XRD) was used to detect phase separation and crystallization of 1.5, 2.0, 2.5, and 4.0 nm HfSiON films after 1000 °C 10 s dopant activation anneal. Crystallization peaks corresponding to monoclinic and tetragonal HfO2 were detected in 2.5 and 4.0 nm HfSiON films. These GI-XRD results were supported by plan-view transmission electron microscopy images of the HfSiON films. Film crystallinity seems to impact voltage instability in thicker HfSiON films.