Ion Beam Synthesis and Characterization of Crystalline Si3N4 Surface Layers

A thin Si3N4 surface layer is formed by implantation of 60 keV 15N nitrogen ions into single-crystalline silicon <100> with a fluence of 5.6x1017 ions/cm2 and subsequent annealing (1295°C, 15 min) under high vacuum conditions. The 15N depth distribution is measured with the resonant nuclear reaction 15N(p,alpha-gamma)12C. The formation of Si-N bonds is proven by Fourier transform infrared spectroscopy using samples implanted with 14N ions and 15N ions, respectively. The crystallinity of the Si3N4 surface layer is studied by X-ray diffraction and transmission electron microscopy. The annealing process leads to the formation of a polycrystalline alpha-Si3N4 surface layer with a thickness of 90 nm. The analysis of high resolution TEM micrographs shows that the layer is split into two sublayers both consisting of single alpha-Si3N4 crystals with lateral extension up to 500 nm.