| Sol-gel methods for fabricating ceramic membranes on porous supports include dip coating, evaporative drying, and sintering. The ceramic membranes of interest in the present research were prepared from aqueous sols of silica, titania, or iron oxide nano-particles which were deposited on porous alumina supports. Physisorption measurements indicate that the diameters of the pores in the resulting membranes are 20 A or smaller. Defect formation during fabrication is particularly problematic for ceramic membranes with pore diameters in the nanometer range. Solutions to these problems would greatly enhance the commercial potential of nano-filtration membranes for gas-phase separations.;Cracks are debilitating defects which originate during the drying and firing phases of fabrication. As water evaporates during drying, the sol-gel film is subjected to large capillary forces. Unchecked, these tensile forces result in catastrophic cracking across the membrane. A novel technique called internal deposition can be employed to deposit the sol particles within the pores of the support rather than on its surface. Internal deposition obstructs the propagation of cracks, thereby reducing the impact of crack-type defects. A patent for demonstration of proof of concept of the internal deposition technique has been received. Experimental difficulties associated with the nonuniform morphology of the tubular alumina support hindered further development of the internal deposition protocol.;The final phase of the research incorporated a support containing uniform capillaries (Anotec(TM) disks). Two-level factorial experiments were conducted to determine the effects of various deposition and drying conditions (viz., speed and method of deposition, surface charge, humidity, and drying rate) on membrane performance. Membrane performance was characterized in terms of the permeabilities of nitrogen and helium in the resulting membranes. The permeability and pressure data were incorporated in a transport model to characterize the mechanisms of fluid flow and the morphologies of the membranes. Electron microscopy was employed to evaluate membrane coverage and to identify defects in the membranes. The results of the factorial experiments indicate that membrane performance is strongly affected by humidity during deposition and drying. These results underscore the importance of controlling process humidity during fabrication of ceramic membranes. |
