In a first series of experiments, nano-sized TiO₂-ZrO₂ membrane materials were prepared by a polymeric sol-gel route and their properties were investigated by dynamic light scattering (particle size), N₂-adsorption (pore size) and XRD (phase structure). The composition with the TiO₂:ZrO₂ ratio of 1:1 exhibited the most promising characteristics including a particle size of ~3-6 nm, a microporous structure with a pore size <1 nm and an amorphous phase up to 600 °C.

In a second series of experiments, these membrane materials were coated on an alumina membrane carrier consisting of a macroporous α-Al₂O₃ substrate and a mesoporous γ-Al₂O₃ membrane layer with a pore size of 5 nm. Structural examination of the TiO₂-ZrO₂ membranes by high resolution SEM and TEM showed very homogeneous top layers with a thickness of ~30-50 nm. The gas permeation of the top layer was investigated by standard gas permeation tests with He, H₂, CO₂ und N₂. The results were compared with data obtained for microporous SiO₂ membranes which were coated on the same substrate. The SiO₂ membranes showed 100 % H₂/CO₂ separation which indicated the formation of high quality layers by our clean room dip-coating procedure. The novel TiO₂-ZrO₂ layers were much tighter and showed a H₂/CO₂ permselectivity of ~10 with very low fluxes. Current investigations are aimed to enhance this performance by synthesis adaption.

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