We synthesized Ta3N5 by ammonolysis of Ta(OH)5. Ta(OH)5 was prepared by titration using TaCl5. The stirring speed and the amount of NH4OH to be added were important factors for controlling the particle size and formation of Ta(OH)5 during titration. During transformation of Ta(OH)5 to Ta3N5, the color changed from white to red. A small particle size and high level of formation of Ta(OH)5 improved nitridation, which was related to the color value. An x-ray diffractometer was used for phase identification. A scanning electron microscope was used to determine the microstructure, particle shape, and size. A colorimeter was used to obtain CIELab values. Ultraviolet–visible (UV–VIS) spectroscopy was carried out to determine the absorbance of colored powders. Thermogravimetry and a differential scanning calorimeter were used in air with a heating rate of 5 °C/min for thermal stability and behavior. An ON detector was used for detecting oxygen and nitrogen contents in Ta3N5.