4. Conclusions
A nano-composite ceramic membrane with a graded structure was successfully synthesized to purify hydrogen at high operating temperatures. This membrane was prepared by depositing a dual element thin layer composed of SiO2 and Al2O3 on top of a graded substrate by co-current CVD method. The graded substrate was synthesized by dip-coating the macroporous α-alumina support with three different size controlled boehmite sols using sol–gel method. Boehmite sols of different particle size in the range of 50–700 nm were obtained by carefully hydrolysis of aluminum tri isopropilate followed by peptization with nitric acid. It was found that the hydrolysis time and acid concentration would affect sol particle size, so that longer hydrolysis time and lower acid concentration gave larger particle size which was supposed to be related to the formation of larger agglomerates in sols. SEM images obtained from cross section of the membrane indicated formation of a multilayer structure with an intermediate thickness of about 2.5 μm and a top selective layer of 80–100 nm. Permeation tests showed a reduction in gas permeance values after 6 h of CVD, but H2/N2 selectivity increased from 5.6 to a high value of 203. This happens because gas permeation mechanism changes from Knudsen diffusion in intermediate layer to an activated mechanism of hopping between solubility sites in dense top layer.