Ytterbium monosilicate (Yb2SiO5) powder was successfully synthesized by the solid-state diffusional process at a low temperature (1350 °C) to serve as an environmental barrier coating (EBC). The stabilization procedure of the synthesized powder in the spray drying process was also presented. The synthesized monosilicate powder was used as a starting material in the EBC development. Ytterbium monosilicate coating was applied on the SiC/C ceramic composite substrate using the conventional atmospheric plasma spray (APS) technique. XRD analysis of the synthesized powder after the spray drying process showed a complete reaction between silica (SiO2) nanoparticles and ytterbium oxide (Yb2O3), leading to the formation of Yb2SiO5 without any side-product. Powder morphology, the corresponding elemental analysis of the spray-dried powder, and the microstructure of monosilicate coatings on the SiC/C substrate were investigated by the scanning electron microscopy (SEM). The particle size distribution of the spherical powder was found to be in the range of 20–80 μm. The thickness of the Yb2SiO5 coating was also in the range of 60–70 μm.