Permporometry characterization of microporous ceramic membranes

An evaluation of nano-order pore size of membranes was carried out using permporometry, the basic principle of which is based on capillary condensation of vapor and the blocking effect of permeation of a non-condensable gas. A computer-controlled apparatus was constructed, where liquid was injected by a syringe pump and nitrogen was used as a carrier, and was applied to the evaluation of the pore size of ceramic membranes prepared from a silica–zirconia composite. The pore size distribution, based on the Kelvin equation (Kelvin diameter), was evaluated over a range of 0.5–30 nm, using water as a condensable vapor. Vapors used in the present study were water, methanol, ethanol, isopropanol, carbon tetrachloride, and hexane. For the case of relatively large pore sizes (larger than 1 nm, based on water vapor), pore size distribution obtained by water vapor agreed very well with those by carbon tetrachloride and hexane. However, pore sizes measured using alcohols were found to be smaller than those determined by water vapor. For the case of pore sizes smaller than 1 nm, the adsorption layer before capillary condensation appears to play an important role.