This project is aimed at synthesis of a new inorganic dual-phase carbonate membrane for high temperature CO2 separation. Metal-carbonate dual-phase membranes were prepared by the direct infiltration method and the synthesis conditions were optimized. The dual-phase membranes are gas-tight with helium permeance about six orders of magnitude lower than that for the metal support. Efforts were made to test seals for permeation and separation experiments for dual-phase membrane at the intermediate temperature range (about 500 degrees C) under oxidizing atmosphere. An effective new permeation cell with a metal seal was designed, fabricated and tested. The permeation setup provided leak-free sealing for the dual-phase membranes under the desired operation conditions. Though the reliable data showing high permeance for carbon dioxide with oxygen for the prepared metal-carbonate dual phase membrane has not been measured, the research efforts in improving membrane synthesis and setting up a new permeation cell with suitable seal have made it closer for one to demonstrate good dual-phase membranes for high temperature carbon dioxide separation. Research efforts were also directed towards preparation of a new ceramic-carbonate dual- phase membrane. Porous lanthanum cobaltite (LC) perovskite type oxide ceramic support with oxidation resistance better than the metal support and high electronic conductivity (1300-1500 S/cm in 400-600 degrees C), was prepared and studied as an alternative support for the dual-phase carbonate membranes. The LC powder was found not reactive with the carbonate at 600 degrees C. The porous LC disks have helium permeance and pore diameter smaller than the metal support but larger than the common a-alumina support. These results show promise to use the LC support for preparation of oxidation resistant dual-phase carbonate membranes.