The scope of this thesis is to design defect-free microporous and mesoporous ceramic membranes having micro-engineered pore network that would contribute to the enhancement of pore control abilities as well as the thermal stability.In this study, mono-dispersed silica sols having well-defined silica spheres ranging in size from 5 to 700 nm were prepared through sol-gel methods and thin membrane layers were consolidated on either y-alumina support or unsupported form.The packing of 5 nm silica spheres resulted in micropores of 0.87 nm in 400 oC treatedmembranes with the porosity of 0.32 which are in well aggrement with the porosity level of random loose packing. Silica spheres with varying concentration and size were incorporated into polymeric network to complement the percolative structure of sphere packing with interpenetrated polymeric silica network in order to design well-defined thermally stable transport pathway. Low shrinkage value was obtained for sphere incorporated system providing the high thermal stability by affecting the thermally induced microcrack formation as well as the structural relaxation during consolidation.The resulting hybrid structure enabled the detailed transport properties that support to be able to control the pore structure but N2/CO2 separation properties are needed to be improved.Stable polymeric alumina sols having particle sizes smaller than 2 nm could be obtained when the hydrolysis conditions were accurately controlled. The mixture of prepared polymeric silica and alumina sols in mullite compositions (3:2) provided to the crystallization of mullite with homogeneously mixed stable oxide network upon heat treatment at 775 oC.