Freeze‐dry processing was investigated as a means of producing homogeneous multicomponent preceramic powders. A general procedure was developed for synthesizing homogeneous multicomponent powders by spray freezing and subsequent freeze‐drying. Uniform particle morphology and high chemical homogeneity were used as criteria for powder quality. Methods of controlling powder morphology and sources of chemical segregation within the powder processing scheme were determined and classical transport phenomena models were constructed in order to define operating parameters required to meet powder quality specifications.