Studies of the mechanisms by which cerium dioxide enhances automotive catalyst performance would be facilitated by the use of pure, high‐surface‐area forms of cerium dioxide. A cerium dioxide powder with a BET area of 50 m 2 ·g −1 has been prepared by spray drying an aqueous solution of cerium nitrate, citric acid, and nitric acid. The thermal stability of the BET area at temperatures from 500° to 1100°C has been determined and compares favorably to other CeO 2 powders. Microstructure evolution during thermal treatments is discussed and pelleting procedures are reported.