Morphology, structure, chemical composition, and light emitting properties of very thin anodic silicon films fabricated using short single pulses of current

In this work, the morphology, structure, surface chemical composition, and optical properties of very thin (10-70 nm) anodic silicon films grown on a silicon substrate by electrochemical dissolution of bulk crystalline silicon in the transition regime between the porous formation and electropolishing were investigated in detail. Anodization was performed by using short single pulses of anodization current in low and high hydrofluoric acid (HF) concentration electrolytes. A systematic comparison was made between films grown at low and high HF concentration electrolytes. The morphology and structure of the films were investigated by combining atomic force microscopy and transmission electron microscopy (TEM), while x-ray and ultraviolet photoelectron spectroscopies were used to investigate the chemical composition of the films. Photoluminescence was used to investigate the optical properties. It was found that films that formed at low HF concentrations were much thinner than films that formed at high HF concentrations due to surface dissolution of the films during anodization. High resolution TEM images revealed an amorphouslike structure (porous) in all of the films in which discrete Si nanocrystals (NCs) were identified. NC size was, on the average, larger in films fabricated in low HF concentration electrolytes and these films were not luminescent. On the other hand, films fabricated in high HF concentration electrolytes were thicker and contained smaller NCs. A silicon oxide layer covered the internal surface of all films, this oxide being much thinner in films grown at high HF concentrations. This last effect was attributed to self-limiting oxidation of the very small NCs constituting these films.