Dielectric resonators are widely used as components of microwave resonant cavi- ties with high dielectric constant, high quality factor and low temperature dependent resonant frequency. Recent advances in the synthesis of materials find several methods of preparation that includes microwave processing. It is possible to use the microwave for the synthesis of materials in two ways. Once the calcination of the required material is performed with conventional fur- nace, the microwave assisted sintering can be used for more densification. The other way is to directly use the microwave assisted process for obtaining the densified pellets from the stoichio- metrically mixed starting reagents. In this paper, we report the synthesis of Sm(Zn0.5Ti 0.5)O3 and ZnO-TiO2 using conventional sintering, microwave assisted sintering and microwave assisted synthesis. Phase formation was observed with XRD and surface morphology was observed using AFM. Microwave dielectric properties of all these systems were obtained using Hakki-Coleman method and cavity resonance method. The paper analyzes the variation between the microwave dielectric property and surface morphology of the above two systems synthesized by the three different routes. Copyright © (2008) by the Electromagnetics Academy.