In this work, a tin-gold layer was deposited on porous silicon (KEF 100) substrates by vacuum-thermal process (VUP) to improve the performance of sensors. By the method of X-ray photoelectron spectroscopy (XPS) we analyzed  the surface of the materials of the original porous silicon, as well as porous silicon with tin and gold, according to the method [1]). XPS overview spectra allow identifying elements present on the sample surface, as well as determining  their oxidation state and concentration. Using this information, valuable data on the surface composition can be obtained and the chemical structure of the sample can be analyzed. The results obtained showed that  using the vacuum-thermal method can be successfully applied to obtain nanocomposites of porous silicon with tin and gold. The obtained nanocomposites contain phases of tin dioxide, tin suboxide/monoxide and metallic tin.  Compared to tin, the gold film is formed in a smoother, more uniform manner. XPS spectra show that the gold is metallic, free of impurities and oxides.