The fabrication of diamond-based optical elements for high-power CO 2 lasers is of particular interest because of low optical absorption, high thermal conductivity and weak temperature dependence of the refractive index of diamond. In earlier publications, we presented the results of the implementation of ion-chemical etching technology for generating a diffraction grating on the surface of a diamond film. The results on generating diamond diffractive optical elements and a sub-wavelength antireflection structure by plasma etching were also presented. In this paper, we study the generation of the grating on the diamond surface by ion-chemical etching. The choice of (Ar+O 2) mixture as a working gas and use of niobium as a masking layer are substantiated. The results of studying a diffraction microrelief generated on the diamond-film surface through ion-chemical etching are discussed.