Eucryptite spheres with average diameters in the range 40-60 mu m were synthesized using a newly developed sol-emulsion-gel approach. Unlike the conventional method, emulsions were prepared with aqueous powder suspensions. With this scheme, a large-scale production of eucryptite spheres, from suspensions with a solid content of 50-60wt%, is readily straightforward. We found that emulsions are formed in a narrow synthesis range determined by the large number of experimental parameters such as the composition of the suspension, the type/amount of the organic solvent and of the surfactant. Although the formation of eucryptite spheres is sensitive to a small variation in these parameters, we have established optimal synthesis conditions for their formation.