Using cellulose triacetate as an added complementary coating material in preparing sustained-release ethylcellulose-cellulose triacetate microcapsules of theophylline, three microencapsulation techniques were investigated. Ethylcellulose-cellulose triacetate composite microcapsules, ethylcellulose-cellulose triacetate dual-walled microcapsules and ethylcellulose microcapsules containing cellulose triacetate matrices were prepared using the non-solvent addition phase separation method. The effects of cellulose triacetate on the release of theophylline from the different ethylcellulose-cellulose triacetate microcapsules were obtained from dissolution studies. The results showed that the release rates of ethylcellulose-cellulose triacetate microcapsules were slower than those obtained from the ethylcellulose microcapsules prepared with similar core to wall ratios. The ethylcellulose microcapsules containing cellulose triacetate matrices had longer release half-times and smaller surface areas than the other capsule preparation. The release patterns of theophylline from the different ethylcellulose-cellulose triacetate microcapsules fitted first-order kinetics. Scanning electron micrographs showed that the surfaces of various ethylcellulose-cellulose triacetate microcapsules were different from those of theophylline, cellulose triacetate matrices of cellulose triacetate microcapsules, and that the surface morphology of ethylcellulose-cellulose triacetate microcapsules was affected by the preparative method.