The paper considers the gas nitriding process with cyclic alternation of atmospheres: ammonia and an ammonia mixture with air for strengthening the corrosion-resistant high-alloyed steel 03Cr11Ni10Mo2Ti, designed to operate at cryogenic temperatures. The formation in steel of a nitrided layer of 130—150μm thickness with increased microhardness (more than 12GPa) is shown experimentally. During the final stage in the ammonia and air environment, iron oxides remain in the compound zone, and a sharp drop in hardness is observed at the border of the core. At the completion of the cyclic process with the stage of saturation in ammonia, a nitrides zone is formed based on the γ′-phase, the layer thickness increases (up to 180(…200μm) and the microhardness profile is smoothed, which reduces the risk of embrittlement.