RESUMO
Single-phase tungsten-doped lanthanum molybdenum oxide (La2MoWO9) ceramic powders were synthesized using the complex polymerization technique. Porous ceramic pellets were obtained by thermally removing graphite, which served as a pore former. The porous pellets were then impregnated with molten eutectic lithium-sodium-potassium carbonates. The energy dispersive X-ray analysis and scanning electron microscopy (FEG-SEM) images of the external and fracture surfaces of the La2MoWO9-(Li,Na,K)2CO3 composite dual-phase membrane revealed the percolation of the carbonate mixture through the pores. Electrochemical impedance spectroscopy measurements conducted at temperatures below and above the melting point of the eutectic carbonate composition demonstrated the contributions of oxygen and carbonate ions to the ionic conductivity of the dual membrane. The electrical conductivity of the carbonate ions within the membrane was continuously monitored for over 1300 h with negligible degradation, implying that the membrane could be used for long-term monitoring of CO2 without aging effects. A comparison of FEG-SEM images taken before and after this endurance test suggested minimal fouling, indicating that the membrane could potentially replace similar zirconia- and ceria-based composite membranes.
RESUMO
An experimental setup for the evaluation of permeation of gaseous species with the possibility of simultaneously collecting electrochemical impedance spectroscopy data in disk-shaped ceramic membranes was designed and assembled. It consists of an alumina sample holder with thermocouple tips and platinum electrodes located close to both sides of the sample. Water-cooled inlet and outlet gas connections allowed for the insertion of the sample chamber into a programmable split tubular furnace. Gas permeation through a ceramic membrane can be monitored with mass flow controllers, a mass spectrometer, and an electrochemical impedance analyzer. For testing and data validation, ceramic composite membranes were prepared with the infiltration of molten eutectic compositions of alkali salts (lithium, sodium, and potassium carbonates) into porous gadolinia-doped ceria. Values of the alkali salt melting points and the permeation rates of carbon dioxide, in agreement with reported data, were successfully collected.