Characterization of porous silicon prepared by powder technology

In this study, we have proposed the powder technology as new method for preparation of bulk porous silicon. Formation of porous silicon by high-energy ball milling followed by pressing and sintering was studied by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy (XPS). A crystalline wafer with (1 1 1) orientation was extensively ball milled up to 72 h leading to a decrease in average crystallite size up to 15 nm. The most significant reduction of crystallite size was observed after milling process for about 24 h. The nanopowders were then pressed into pellets at a pressure up to 400 MPa and sintered at 1173 K for 60 min in a high purity argon atmosphere. Results showed that after sintering the material became porous with uniform porosity in whole volume, independently of the sinter size. It is not possible to prepare such porous materials using the conventional electrochemical etching, where the porous structure depth usually does not exceed tens of micrometers. Core-level XPS studies showed very good agreement between peak positions of the sintered porous silicon and in-situ prepared polycrystalline 20 nm-Si thin film or single-crystalline Si (1 1 1) wafer. Furthermore, the valence band spectra measured for sintered samples are broader compared to those measured for the Si (1 1 1) wafer or polycrystalline Si thin film. On the other hand, the shape and broadening of the valence bands measured for the sintered samples are in very good agreement with those reported for electrochemically prepared porous silicon.