Abstract: In this work, we report on an investigation of the ytterbium diffusion characteristics in lithium niobate. Ytterbium-doped substrates were prepared by in-diffusion of thin metallic layers coated onto x-and z-cut congruent substrates at different temperatures. The ytterbium profiles were investigated in detail by means of secondary neutral mass spectroscopy, optical microscopy, and optical spectroscopy. Diffusion from an infinite source was used to determine the solubility limit of ytterbium in lithium niobate as a function of temperature. The derived diffusion parameters are of importance for the development of active waveguide devices in ytterbium-doped lithium niobate.