ABSTRACTBarium yttrium cuprate powders were prepared by a sol-gel emulsion process in which an aqueous nitrate solution containing Ba, Y, and Cu in the correct stoichiometry was emulsified in heptane. The resulting micrometer-sized droplets were gelled by adding a high-molecular-weight primary amine that extracts nitric acid from the aqueous phase and raises the pH of the droplets. Thermal gravimetric analysis revealed that the correct overall stoichiometry was obtained at temperatures lower than 400 °C during calcination, but X-ray diffraction showed that calcination at temperatures greater than 800° may be required to produce the correct phase. One possible advantage of this technique is the control of powder morphology on a micrometer scale so that powders can be prepared for advanced ceramics processing methods. Also, segregation of components, if any, will be restricted to distances less than one micrometer.