A comparative comparison of the hydrophobicity and surface properties of metal samples obtained by solid-state hydride synthesis (SHS) of metals and layering of different-sized molecules (LDM) of ammonium and organosili-con compounds has been carried out. It was found that the dispersed metal products of SHS are significantly more hydrophobic (on average, by an order of magnitude) compared to metals modified in vapors of industrial water re-pellents. It has been established that among the metal products of SHS based on nickel, copper, and iron with a carbosiloxane nanofilm on the surface, the samples based on iron are the most hydrophobic and heat-resistant in air. The most hydrophilic and chemically active samples were nickel-based, which had a fairly developed surface (about 50 m2/g). The revealed patterns of regulation of the surface properties and hydrophobicity of metal synthesis products are associated with the strongest interatomic metal-silicon chemical interaction in the surface layer of iron-based samples, confirmed by XPS spectroscopy. When a metal product is obtained by successive reduction of the initial sol-id-phase raw material (ore) in methyldichlorosilane (MDCS) vapor and in a methane stream, MDCS performs the functions of a reducing agent and modifier of the metal surface. The metal at the time of appearance, being in a reducing medium, has a reactive surface and actively interacts with MDCS molecules containing chemically stable Si-C groups, with the formation of a strong chemisorption bond between the metal and the protective carbosilox-ane film formed during synthesis, no more than 4–5 nm. Such a mechanism of the process under SHS conditions makes it possible to carry out the reduction and useful modification of the metal within the framework of a single techno-logical process and in one reactor. This research paper was recommended for publication by the organizing com-mittee of the International Conference on Nanophysics and Nanomaterials, 24-25 November 2021, Saint Petersburg, Mining University. © 2022, Ore and Metals Publishing house. All rights reserved.