To overcome the difficulty of preparing the stoichiometric single phase calcium phosphate materials, ultrasonic spray pyrolysis was used to fabricate various calcium phosphates. Effect of the initial Ca/P ratios and pyrolysis temperature were investigated in preparation of single phase materials. Also thermal stability of the obtained powders was estimated with the heat treatment in the air. Crystallinity of the powders was analyzed using XRD and FT-IR. The HAp and β-TCP powders with single phase could be obtained from their stoichiometric Ca/P ratios of 1.50 and 1.67, respectively. These single phase powders with good crystallinity and stoichiometry were stable with respect to heat treatment up to 1000oC. The particle size of these powders would be controlled by the concentration of starting solution.