CNx/TiNy multilayers have been prepared by ion beam sputtering and analyzed by X-ray diffraction, transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray and X-ray photoemission spectroscopy. The structure analyses shows that the films may contain several different kinds of C-N crystals embedded in the amorphous matrix. These crystals have hexagonal and cubic crystalline structures. The TiNx layer in multilayers is primarily amorphous and contains only a few dispersed Ti2N crystals. The thickness of CN, and TiNy layers in the CNx/TiNy multilayers is about 20 and 30 nm, respectively. The atomic ratios of [N]/([C] + [N] + [Til) in the multilayers vary from 20 to 41 at%. The bonding ratios of C - N/C = N of the CN, layer in multilayers reach 0.447 or 0.585 as calculated from the C1s and N1s X-ray photoemission spectra, respectively.