Yttrium aluminum garnet doped with ytterbium (YAG:Yb) ceramic powders were synthesized using the chemical precipitation method, from which optical ceramic samples were fabricated. Dispersants, namely polyvinylpyrrolidone and ammonium sulfate, were employed during powder synthesis, washing, and milling. The results presented include data on the phase composition, specific surface area, scanning electron microscopy, and particle size distribution of the ceramic powders. It was noted that the addition of polyvinylpyrrolidone and ammonium sulfate to the reaction mixture, as well as to the washing and milling solutions, alters the particle size distribution and specific surface area of the powders, while also influencing the kinetics of phase transformations. Furthermore, the influence of these dispersants on the optical properties of YAG:Yb ceramics and the number of macrodefects was revealed.